Document QkmEmjBXVZLnmnbDDOb3ynyqo

This information is an attachment to the restriction proposal for PFAS (appendix to Annex E.4) and compiles an The aim with this overview is to summarize relevant analytical methods for the analysis of PFASs in several matric Various sources of information have been investigated including recent peer-reviewed literature (2010-2022) and Information on analytics of relevant publications and standards were extracted in this excel sheet. Extracted info Please note: 1. Every matrix discussed in the report has an extra tab. Publications or standards which could be assigned to mo 2. Application notes of laboratories can be found in a seperate tab (as they usually can not be assigned to specific 3. Sorting of the respective columns is possible (for example by year). 4. Standard methods are highlighted in green and are therefore easy to find. 5. The same notation (for e.g., PFAS, methods) was used as in the literature. nalytical methods available for different matrices. ices, including products wherein PFASs are often used, like textiles and food-contact materials etc. d well-established standards. Additional, application notes from laboratories were collected. rmation include sampling, pre-treatment, extraction, clean-up, measurement, quantification, LoD et ore than one category can be found in each respective tab. ific matrices). Title Authors CEN/TS 15968:2010 - Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LCqMS or LC-tandem/MS Post-Chromatographic Dicationic Ionic Liquid-Based Charge Complexation for Highly Sensitive Analysis of Anionic Compounds by Ultra-High-Performance Supercritical Fluid Chromatography Coupled with Electrospray Ionization Mass Spectrometry Li et al. Determination of perfluorooctanoic acid and perfluorooctane sulfonate by automated in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry Saito et al. Removing perfluorooctane sulfonate and perfluorooctanoic acid from solid matrices, paper, fabrics, and sand by mineral acid suppression and supercritical carbon dioxide extraction Chen et al. Concentrations and trends of perfluorinated chemicals in potential indoor sources from 2007 through 2011 in the US Liu et al. Determination of Perfluorinated Compounds (PFCs) in Various Foodstuff Packaging Materials Used in the Greek Market. Zafeiraki et al. Determination of fluorotelomer alcohols in selected consumer products and preliminary investigation of their fate in the indoor environment Liu et al. Emission of perfluoroalkyl carboxylic acids (PFCA) from heated surfaces made of polytetrafluoroethylene (PTFE) applied in food contact materials and consumer products Schlummer et al. Poly- and perfluoroalkyl substances (PFASs) in indoor dust and food packaging materials in Egypt: Trends in developed and developing countries Shoeib et al. The last straw: Characterization of per- and polyfluoroalkyl substances in commercially-available plant-based drinking straws Timshina et al. Polyfluorinated surfactants (PFS) in paper and board coatings for food packaging Trier et al. (b) Polyfluoroalkyl phosphate esters and perfluoroalkyl carboxylic acids in target food samples and packaging--method development and screening Gebbink et al. Perfluoroalkyl and polyfluoroalkyl substances in consumer products Kotthoff et al. Closing the Mass Balance on Fluorine on Papers and Textiles Robel et al. In-Vial Extraction Large Volume Gas Chromatography Mass Spectrometry for Analysis of Volatile PFASs on Papers and Textiles Rewerts et al. How Do We Measure Poly- and Perfluoroalkyl Substances (PFASs) at the Surface of Consumer Products?: Environmental Science and Technology LETTERS Tokranov et al. Ubiquitous Occurrence of Fluorotelomer Alcohols in Eco-Friendly Paper- Made Food-Contact Materials and Their Implication for Human Exposure. Yuan et al. Total Fluorine Measurements in Food Packaging: How Do Current Methods Perform? Schultes et al. Fluorinated Compounds in U.S. Fast Food Packaging Schaider et al. An exploratory analysis of poly- and per-fluoroalkyl substances in pet food packaging from the United States Chinthakindi et al. Migration of perfluoroalkyl acids from food packaging to food simulants Xu et al. PFOA and PFOS Levels in Microwave Paper Packaging between 2005 and 2018. Monge Brenes et al. Occurrence of per- and polyfluorinated compounds in paper and board packaging materials and migration to food simulants and foodstuffs Zabaleta et al. Screening and identification of per- and polyfluoroalkyl substances in microwave popcorn bags Zabaleta et al. Method foranalysis of 68 organic contaminants in food contact paper using gas andliquid chromatography coupled with tandem mass spectrometry Vavrous et al. Significance of Perfluoroalkyl Substances (PFAS) in Food Packaging Curtzwiler et al. Fast determination of perfluorocompounds in packaging by focused ultrasound solid-liquid extraction and liquid chromatography coupled to quadrupole-time of flight mass spectrometry Moreta et al. Determination of perfluorinated alkyl acids in corn,popcorn and popcorn bags before and after cooking by focused ultrasoundsolid-liquid extraction, liquid chromatography and quadrupole-time offlight mass spectrometry, Moreta et al. An Optimized Method for the Determination of Perfluorooctanoic Acid, Perfluorooctane Sulfonate and Other Perfluorochemicals in Different Matrices Using Liquid Chromatography/Ion-Trap Mass Spectrometry Dolman et al. Tools to discover anionic and nonionic polyfluorinated alkyl surfactants by liquid chromatography electrospray ionisation mass spectrometry Trier et al. (a) Determination of perfluorooctane sulfonate and perfluorooctanoic acid in food packaging using liquid chromatography coupled with tandem mass spectrometry Poothong et al. Analysis of per- and polyfluorinated substances in articles Blom et al Analysis of PFASs and TOF in products Borg et al. Per- and Polyfluorinated Alkyl Substances (PFAS) in Paper and Board Food Contact Materials--Selected Samples from the Norwegian Market 2017 Granby et al. PIGE as a screening tool for Per- and polyfluorinated substances in papers and textiles Ritter et al. Determination of Selected Perfluorinated Acids (PFCAs) and Perfluorinated Sulfonates (PFASs) in Food Contact Materials Using LCMS/MS Determination of perfluorocompounds in popcorn packaging by pressurised liquid extraction and ultra-performance liquid chromatography-tandem mass spectrometry Surma et al. Martnez-Moral et al. Fast and simple determination of perfluorinated compounds and their potential precursors in different packaging materials Zabaleta et al. Comprehensive analysis of photoinitiators and primary aromatic amines in food contact materials using liquid chromatography High-Resolution Mass Spectrometry Sanchis et al. Selective and sensitive analysis by reactive easy ambient sonic-spray ionization: Synergistic combination of non-polar spray solvent and dicationic ionic liquid Lv et al. Impact of household cooking on release of fluorinated compounds PFOA and PFOS from Tefal coated cookware to foods AbulFadl et al. CEN/TS 15968:2010 - Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LCqMS or LCtandem/MS Journal year Comments DOI link Anal Chem Also used for other matrices, sample 2010 treatmant different 2021 Method development 10.1021/ acs.analchem.0c04612 Anal Chim Acta Chemosphere Low relevance due to 2010 focus on migration 10.1016/ j.aca.2009.11.004 2012 Method development 10.1016/ j.chemosphere.2012.0 6.003 Chemosphere Chemosphere 2014 na 10.1016/ j.chemosphere.2013.1 0.001 Reference taken from Al Amin-Review 2020, From 2014 Ramrez Carnero 2021 https://doi.org/10.1016 Chemosphere 2015 na 10.1016/ j.chemosphere.2014.0 6.012 Chemosphere Low relevance due to 2015 focus on emission 10.1016/ j.chemosphere.2014.1 1.036 Chemosphere Chemosphere Reference taken from 2016 AlAmin-Review 2020 10.1016/ j.chemosphere.2015.0 8.066 Modified version of US EPA's NRMRL Solids Extraction Protocol for PFAS Isotope Dilution 2021 Analysis 10.1016/ j.chemosphere.2021.1 30238 Environ Sci Pollut Res Int 2011 From Zafeiraki 2014 10.1007/s11356-0100439-3 Environ Sci Pollut Res Int 2013 na 10.1007/s11356-0131596-y Environ Sci Pollut Res Int 2015 na 10.1007/s11356-0154202-7 Environ Sci Technol Mass balance between 10.1021/ 2017 PIGE and other methods acs.est.7b02080 Environ Sci Technol 2018 na 10.1021/ acs.est.8b04304 Environ Sci Technol Lett Method development for 10.1021/ 2019 consumer products acs.estlett.8b00600 Environ. Sci. Technol From Ramrez Carnero 2016 2021 https://doi.org/10.1021 Environmental Science & Technology Letters 2019 na 10.1021/ acs.estlett.8b00700 Environmental science &amp; technology letters 2017 na 10.1021/ acs.estlett.6b00435 Environmental Technology and Innovation 2021 na https://doi.org/10.1016 Food Addit Contam Part A Chem Anal Control Expo Risk Assess 2013 na 10.1080/19440049.20 13.789556 Food Addit. Contam. Part B https://doi.org/ From Ramrez Carnero 2021, used method 10.1080/19393210.20 19.1592238 developed by Moreta et al. 2019 2014 Food Chem according to method developed by Zabaleta 2017, also including 2020 migration 10.1016/ j.foodchem.2020.1267 46 Food Chemistry Reference taken from 2017 AlAmin-Review 2020 https://doi.org/10.1016 FoodControl 60 2016 From Sanchis 2017 https://doi.org/10.1016 Integrated environmental assessment and management 2021 Method development 10.1002/ieam.4346 J Chromatogr A 2013 na 10.1016/ j.chroma.2013.06.024 J. Chromatogr. A 2014 CAS from Sanchis 2017 https://doi.org/10.1016 J. Chromatogr. B From Ramrez Carnero 2011 2021 and Zafeiraki 2014 https://doi.org/10.1016 Journal of chromatography A Method development, 2011 Applied in Trier 2011b 10.1016/ j.chroma.2011.07.057 Journal of hazardous materials 2012 From Zafeiraki 2014 10.1016/ j.jhazmat.2011.12.050 Nordic Council of Ministers 2015 na http://dx.doi.org/10.602 Nordic Council of Ministers 2017 na http://dx.doi.org/10.602 Norwegian Food Safety Authority Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 2018 Also migration measured na 2017 https://doi.org/10.1016 Packaging Technology and Science Talanta 2015 na 2012 From Zafeiraki 2014 10.1002/pts.2140 10.1016/ j.talanta.2012.09.007 Talanta Talanta Talanta Reference taken from 2016 AlAmin-Review 2020 10.1016/ j.talanta.2016.02.022 Low relevance due to focus on photoinitiators/ 2019 primary aromatic amines 10.1016/ j.talanta.2018.08.047 Method development with PFOA, PFOS as model 10.1016/ 2020 analyts j.talanta.2020.120929 World Journal of Advanced Research and Reviews Low relevance due to 2019 focus on migration 10.30574/ wjarr.2019.3.2.0060 Also used for other matrices, sample 2010 treatmant different PFAS CAS (if available in publication) 1763-23-1 (PFOS) PFOS, PFOSA, N-Me-FOSA, N-Et-FOSA, 754-91-6 (PFOSA) N-Me-FOSE alcohol, N-Et-FOSE alcohol, 24448-09-7 (N-Me-FOSE alcohol) 1691-99-2 PFOS salt (N-Et-FOSE alcohol) PFDoA, PFUdA, PFDA, PFna, PFOA, PFHpA, PFHxA, PFPeA, PFOS, PFBS na PFOS, PFOA na PFOS, PFOA na 9 PFCAs (C4 to C12), 5 PFASs (C4, C6, C7, C8, C10) na PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoA, PFBS, PFHxS, PFOS, PFTrDA, PFTeDA, PFHxDA, PFODA, PFDS na 6:2 FTOH, 8:2 FTOH, 10:2 FTOH na PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUna, PFDoA na 6:2, 8:2, 10:2 FTOH, Me-FOSA, Et-FOSA, 6:2 FTMAC, 8:2, 10:2 FTAC, 6:6, 6:8, 8:8 PFPIA, 6:2, 8:2 monoPAPs, 6:2, 8:2 diPAPs, PFOS, PFOA, PFDS, PFBS, PFHxS na 53 semi-volatile PFAS including PFBA, PFOA, PFHxA na Non-targeted: FTOH, monoPAPS, diPAPS, triPAPS, S-diPAPS, SN-diPAPS, Alkyl-PAPS, 3-[2- (perfluoroalkyl)ethylthio] propionate, PFOS, PFSA, PFOSA, PFOSF, Et-PFOSA, Alkyl-PFOSA, Fluoroalkoylate, Fluoroacrylate, PFPE, di (N-ethyl perlfluoroalkyl) N-propanoic acid na PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFTrDA, 4 monoPAPs, 16 diPAPs including 6:2/6:2 diPAP, 8:2/8:2 diPAP, 10:2/10:2 diPAP, 7 triPAPs na PFBA, PFPA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUna, PFDoA, PFTrA, PFTeA, PFBS, PFHxS, PFHpS, PFOS, PFDS, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, PFOSA na total fluorine, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, EtFOSE, C3--C17 PFCAs, C4, C6, C8, C10 n:2 FTCA, C4, C6, C8, C10 n:2 FTUCAs, C3, C5, C7, C9 n:3 FTCA, C2-C10 PFSAs, fluorotelomer sulfonates (C4, 6, 8, 10 FTSAs), fluoroalkyl sulfonamido acetic acids (C4-C8 FASAA), N-methyl fluoroalkyl sulfonamide acetic acids (C4-C8 MeFASAA), ethyl fluoroalkyl sulfonamido acetic acids (C4-C8 EtFASAA), disubstituted perfluoroalkyl phosphinic acids (C4/C4-C8/C8 PFPIA), disubstituted polyfluorinated phosphate esters (C4/ C4-C10/C10 diPAP), fluorotelomer mercaptoalkyl phosphate esters (C6/C6-C10/C10 FTMAP), and ethyl perfluorooctanesulfonamido ethanol- based polyfluoroalkyl phosphate diester (C8/C8 SAmPAP) na 21 volatile PFAS including 4:2, 6:2, 8:2, and 10:2 FTOH, N-MeFOSA, NEtFOSA, N-MeFOSE, and N-EtFOSE na surficial fluorine content, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA, PFBS, PFHxS, PFOS, FOSA, 6:2 FtS, N-MeFOSAA, N-EtFOSAA na 13 PFCAs, 6:2 FTOH, 8:2 FTOH, 10.2 FTOH, 12:2 FTOH, 14:2 FTOH, 16:2 FTOH, 18:2 FTOH na Total fluorine, targeted: PFCAs, C4- C15), PFSAs (C4, C6, C8, C10), FOSA, perfluoroalkane sulfonamidoacetic acids, FTSAs (4:2, 6:2, 8:2), fluorotelomer carboxylic acids (5:3, 7:3, 9:3), ADOna, F53-B, and polyfluoroalkyl phosphoric acid mono- and diesters (mono- and diPAPs) na total fluorine, 89 targeted PFASs including PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFDA, PFUna, PFDoA, PFTriA, PFBS, PFHXS, 4:2 FTS, 6:2 FTS, 10:2 FTS, 6:2-8:2 diPAP, 8:2-8:2 diPAP, C5 polyfluoro ether, C6 polyfluoro ether, 5:3 FTCA, PFHxPA, 6:6 FTMAP, ADOna, FHUEA, nMe-FBSE, nafion CA, PFOSulfinate, GenX, non-targeted na 9 PFCAs namely PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA and 4 PFSAs namely PFBS, PFHxS, PFOS, PFDS na PFBS, PFHxS, PFOS, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA na PFOA, PFOS na Targeted analysis of 23 PFASs including PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, 6:2 monoPAP, 8:2 monoPAP, 6:2 diPAP, 8:2 diPAP, 6:2 FTCA, 6:2 FTUCA, 8:2 FTCA, 8:2 FTUCA, 5:3 FTCA, 7:3 FTCA na PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFPeDA, PFHxDA, 8:2 FTCA, 10:2 FTCA, 8:2 FTUCA, 10:2 FTUCA, 7:3 FTCA, 9:3 FTCA, 5:3 FTUCA, 7:3 FTUCA, 9:3 FTUCA na PFOS, PFBA, PFPeA, PFHxA, PFOA, PFna, PFDA, PFUna, PFDoA, FOSA, PFBS, PFOPA, PFHxS, PFHxPA, PFDPA 1763-23-1 (PFOS) 375-22-4 (PFBA) 2706-90-3 (PFPeA) 307-24-4 (PFHxA) 335-67-1 (PFOA) 375-95-1 (PFna) 335-76-2 (PFDA) 2058-94-8 (PFUna) 307-55-1 (PFDoA) 754-91-6 (FOSA) 29420-49-3 (PFBS) 355-46-4 (PFHxS) PFBA, PFHxA, PFOA, PFDA na PFHpA, PFOA, PFna, PFOS, PFDA, PFUnDA, PFDoA na PFOS, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUna, PFDoA 1763-23-1 (PFOS) 375-22-4 (PFBA) 2706-90-3 (PFPeA) 307-24-4 (PFHxA) 375-85-9 (PFHpA) 335-67-1 (PFOA) 375-95-1 (PFna) 335-76-2 (PFDA) 2058-94-8 (PFUna) 307-55-1 (PFDoA) PFOA, PFHxA, PFHpA, PFna, PFDA, PFUA na Non-targeted: PFCA, PFSA, PFASA, FTOH, monoPAPs, diPAPs, S-diPAPs, Fluoroethoxylate na PFOS, PFOA na PFCAs (PFBA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA), PFASs (PFBS, PFHxS, PFOS), PAPs (6:2 diPAP, 6:2 monoPAP, 8:2 diPAP, 8:2 mono-PAP), FTOH (4:2, 6:2, 8:2), FTS (4:2, 6:2) 375-22-4 (PFBA), 307-24-4 (PFHxA), 375-85-9 (PFHpA), 335-67-1 (PFOA), 375-95-1 (PFna), 335-76-2 (PFDA), 4234-23-5 (PFUnDA), 307-55- 1 (PFDoDA), 72629-94-8 (PFTrDA), 376-06-7 (PFTeDA), 29420-49-3 (PFBS salt), 3871-99-6 (PFHxS salt), 1763-23-1 (PFOS salt), 2043-47-2 (4:2 FTOH), 647-42-7 (6:2 FTOH), 678-39-7 (8:2 FTOH), 57677-95-9 (6:2 diPAP), 57678-01-0 (6:2 monoPAP), 678-41-1 (8:2 diPAP), 5767803-2 (8:2 mono-PAP), 757124-72-4 (4:2 FTS), 29420-49-3 (6:2 FTS) TOF, targeted analysis of PFCAs (PFBA, PFHxA, PFOA, PFna, PFDA), PFSAs (PFBS, PFHxS, PFOS), FTOHs (4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH), FTAs (6:2 FTA, 8:2 FTA, 10:2 FTA), FOSAs (MeFOSA, EtFOSA), FOSEs (MeFOSE, EtFOSE) 375-22-4 (PFBA), 2942049-3 (PFBS salt), 307-24-4 (PFHxA), 3871-99-6 (PFHxS salt), 2043-47-2 (4:2 FTOH), 757124-724 (4:2 FTS), 335-67-1 (PFOA), 1763-23-1 (PFOS salt), 647-42-7 (6:2 FTOH), 29420-49-3 (6:2 FTS), 31506-32-8 (MeFOSA), 4151-50-2 (EtFOSA), 2448-09-7 (MeFOSE), 1691-99-2 (EtFOSE), 375-95-1 (PFna), 335-76-2 (PFDA), 678-39-7 (8:2 FTOH) PFCAs (PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA, PFTeA, PFTrA), PFSAs (PFBS, PFHxS, PFOS, 4H-PFOS, PFDS, PFOSA), monoPAPs (6:2, 8:2), diPAPs (6:2/6:2, 8:2/8:2), FTOHs (4.2, 6:2, 8:2, 10:2) na total fluorine na PFOA, PFOS na PFHpA, PFOA, PFna, PFOS, PFDA, PFUnDA, PFDoA na PFBS, PFHxS, PFOS, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFHxPA, PFOPA, PFDPA, PFOSA, 6:2 FTCA, 8:2 FTCA, 5:3 FTCA, 7:3 FTCA, 6:2 FTUCA, 8:2 FTUCA, 6:2 mono & di PAP, 8:2 mono & di PAP na Post-run target screening analysis of polyfluorinated compounds na PFOA, PFOS na PFOS, PFOA na 1763-23-1 (PFOS) PFOS, PFOSA, N-Me-FOSA, N-Et-FOSA, 754-91-6 (PFOSA) N-Me-FOSE alcohol, N-Et-FOSE alcohol, 24448-09-7 (N-Me-FOSE alcohol) PFOS salt 1691-99-2 (N-Et-FOSE alcohol) Sampling sample amount used Pre- treatment Solids (coated materials): at least 200 cm2 or 2 g, solids (non-coated): sampled according to EN ISO 8130-9 see sampling Sample materials need to ground as appropriate to ensure an efficient extraction process. Textile and paper shall be cut into pieces of maximum 1 cm2 before methanol is added. For grinding of polymers and granulates it is recommended to use EN ISO 6427 or ISO 9113. 32 real textile samples of different fabrics (e.g., cotton, wool, and polyester) and 6 food packaging material samples (e.g., oil-proof hamburger wrapping paper) 1 x 1 cm2, 0.5 g na Surface water and waste water samples, Teflon- coated frying pan from the local market was heating on a cooking stove for 5min after addition of 200mL of distilled water. Aliquots of 0.2 mL of heated water in the frying pan were pipetted into 2-mL autosampler vials and the total volume was made up to 1.0 mL with distilled water. 1 mL filtered (0.2 m nylon syringe) na na na 95 samples from 35 consumer products including carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non- woven medical garments, floor waxes, food- contact paper, membranes for apparel, and thread-sealant tapes. They were purchased from retail outlets in the United States between March 2007 and September 2011. 5 x 5 cm 42 Fast-food packaging, sandwiches, cups, ice cream containers, baking paper, popcorn bags, etc. from Athens market and fast-food restaurants in Greece. 1 cm2 solid products were cut into smaller subsections. Liquid products were subdivided into at least three 30-mL polypropylene vials In the cases when the samples had a printed outside layer, this was removed when possible. Any food content was removed from the packaging, which was then rinsed with ultrapure water to remove salt and dried. 54 consumer products from U.S. open market in the years of 2011 and 2013 (carpet, commercial carpet-care liquids, household carpet/fabric- care liquids, treated apparel, treated home solid samples textiles, treated non-woven medical garments, 0.05 g, liquid floor waxes, food-contact paper, membranes for samples 100 apparel, and thread-sealant tapes) L na 3 PTFE coated pans (claimed to be PFOA free) bought from German stores, 3 waffle irons, Sandwich marker, electric iron, iron sole plate, hair straightener emission analyzed pans pre-cleaned as recommended by their producers Paper and cardboard materials (n=17) constituted fast food sandwiches wrappers for burgers; paper boxes for French fries, pizza sandsandwiches; non-stickbaking cups; microwave bags for popcorn and soup cups.Dust samples were collected from Cairo, Egypt in 2013. The samples were collected from 17 homes, 5 workplaces and 9 cars as obtained from new vacuum cleaner bags. Dust samples from cars were collected from the chairs, the roofs and the dashboards .The dust samples were wrapped in solvent-cleaned aluminum foil and further sealed in polyethylene bags for storage at 4C until processed. Dust: 0.1-0.2 g, FCM: 1/81/4'', < 1 g Dust: sieved, FCM: Removal of the food products, the paper and cardboards were wiped with clean tissue paper, rinsed with deionized water 43 brands of straws (5 plastic, 29 paper, 9 other plant-based) na na 14 papers and board materials intended for contact with food at high temperatures from retailers in Denmark 1 dm2 After removal of the food product, the paper and boards were rinsed for salts with distilled, deionised water. Food contact material that had not been in contact was chosen if possible. Targeted food samples (in their original paper or board packaging materials) were purchased at a Swedish grocery store chain (ICA supermarket) 5 x 5 cm, 5 g and in a McDonald's restaurant in Stockholm in homogenized spring 2012. food sample Food samples that required heating prior to consumption were purchased in duplicates. One portion was analyzed as purchased (hereafter referred to as unprepared food), whereas the other portion was prepared in the microwave oven according to specifications on the packaging materials before analysis (hereafter referred to as prepared food) 115 samples of consumer products including textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes. The individual samples analysed were bought from local retailers or collected by co-workers of the institute or local clubs (e.g. ski waxes from local skiing club). The sampled products span all quality levels from entry level to cutting edge products. The selection of the samples occurred randomly. na na large set of consumer products (food-contact papers, popcorn bag, outerwear textiles, childrens clothing, pillowcase, uhholstery cut from office chair) comprised of paper and textiles purchased by the Washington Department of Ecology in 2015 2 x 2 cm2 (0.3 +/- 0.01 g) cut using methanol-rinsed scissors 7 papers consisted of all new materials purchased or acquired in 2017, including: white copier paper, five food-contact materials, and waterproof notebook paper, 9 textiles consisted of a plain white t-shirt, three office chair upholsteries from the years 1988a, 1988b, and 1993, respectively, an outdoor upholstery purchased in 2017, two articles of previously worn children's clothing (a swimsuit and outdoor vest), and an adult rain jacket purchased in 2015, as well as a piece of a used firefighter's jacket 1.5 x 1.5 cm cut using methanol-rinsed scissors 94 consumer products that represent frequently used items on a college campus of Harvard University. These included: 45 food contact materials, 37 textiles, and 12 domestic products such as lens wipes, bandages, masks, and a shower curtain 1 0.03 g cut using methanol-rinsed scissors, mounted on carbon tape for XPS 69 paper-made FCMs (bags of popcorn, materials labelled as ecological, cupcake packaging, etc.) from Beijing retail market and online. 25 FCMs were purchased from various retail stores in Columbus, Ohio. 0.5 cm x 0.5 cm printed outer surfaces were peeled off from the samples before extraction; for other single-layer samples, the printed portions were cut from the samples before extraction 3 french-fry bags (FF1-FF3) and 6 microwave popcorn bags (MP1-MP6) purchased in Sweden in 2012 5 cm x 5 cm short, samples (5 cm 5 cm) were cut into small pieces, fortified with internal standards (0.5 ng each) 407 samples of paper and paperboard food wrappers and related food packaging at U.S. fast food restaurants (2014, 2015) including food contact paper (e.g., sandwich wrappers and pastry bags), noncontact paper (e.g., outer bags), food contact paperboard (e.g., boxes for fries and pizza), paper cups (for hot or cold drinks), other beverages (e.g., milk and juice PIGE: 2 cm2 containers), with 1 cm2 and miscellaneous (e.g., lids and applesauce hole, MS: 10 containers). cm x 10 cm na .A total of 48 samples (37 packaging and 11 food) from 11 different popular brands of pet (cat and dog) foods marketed in the United States. Of the 37 packaging, 22 were used for cat food, 15 were for dog food. 1 cm2 emptying the contents, packaging material was cut into small pieces The food packaging samples were purchased, unused, directly from local retail food markets. 6 cm 8 cm 0.034 mm, 9.34 g m-2; 3 x 9 cm (migration) na Seven unique unused, unfilled, single-gusseted microwaveprinted popcorn bags were obtained from multiple international suppliers. Three lunch sacks were obtained from three unique retail grocery chains (Ames, IA). The lunch sacks are not printed. ~1.5 g of homogenised sample Sections with the adhesive were removed before sampling, pulverized, suspended (EtOAc) & spiked, mixed; evaporated 12 grease proof P/B packaging materials including a baking paper, a muffin cup, a cardboard plate and a cup, a burger wrapper, two grease proof boxes, two French fries wrappers, two burger clams and a grease proof bag, together with 7 non grease proof materials including two cardboards, two pizza boxes and three cinema popcorn bags were collected randomly from local factories, markets and restaurants between 2018 and 2019. Moreover, microwave popcorn bags were purchased in China (one) and Spain (two) from local supermarkets during 2019. Finally, unprinted pet food paper bags (collected during 2016 and 2018) were also analyzed. 1 cm^2 After removal of the food product, the paper of microwave popcorn bags was rinsed into Milli-Q water. Microwave popcorn bags purchased from Europe (Spain, France, Austria, The Netherlands, Hungary, Germany, Italy, Ireland, Czech Republic, Sweden, United Kingdom and Portugal), America (Mexico, Brazil and United States) and Asia (China and India) during 2015-2016 (all bags were ensured to be manufactured in the corresponding country) 1 dm2, ~1 g removal of the food product, the paper was rinsed for salts with Milli-Q water Real samples of paper FCM were acquired from the market in the Czech Republic 1.0-1.5 g Samples were cut into small pieces (approximately 2 x 10 mm) Strips of unbleached kraft 0.35mm (16 pt) recycled packaging paper 2.54 25 cm were received from a commercial domestic manufacturer and prepared using a JDC Precision sample cutter. 2.54-cm square and two 2.54 ~11.25-cm segments Different food-contact packings like microwave popcorn bag, icecream tub and cardboard cup were obtained from different local supermarkets: 6 microwave popcorn bags, 3 types of microwave popcorn, 5 g cut using methanol-wiped Ti scissors samples were ground Microwave popcorn bags of six different types obtained from local supermarkets in mid-2013 0.50 g, 1.00 g and 1.5 g Before analysis, fat, salt and/or sugar were thoroughly removed from packaging and corn samples with the aid of paper towel, cornand popcorn were sieved through a 0.5 mm mesh sieve. Popcorn bags, baking, paper, box of chips, sandwich wrap, hamburger box from Local shops and fast-food restaurants; bottled drinking water 50 mg na na na na 34 samples of food packaging material made of 5 mm x 5 mm, printing and outside layer of the paper from domestic and international 2 g (dry containers were deliberately removed restaurants in Bangkok, Thailand weight) with the aid of a cutter. In total 29 different samples were analysed. The sampling was concentrated on a few but wide variety of household products, such as cleaning products and polishes for indoor use and for cars and sprays to waterproof shoes or clothes, food contact paper and baking forms included some products less commonly analysed, such as ski wax, dental floss and tablecloths. The samples were purchased in the vicinity of Oslo in supermarket chains that are found all over Norway. depending on the article: 0.05 mL, 71.5100 cm^2 or 0.02-0.16 g vortexing in methanol In total 17 products were randomly selected from shelves in a number of Swedish retail stores and supermarkets for analysis (Cupcake forms, microwave popcorn bag, rinse aid, waterproofing shoe treatment, waterproofing textile treatment, shoe wax, floor polish, furniture polish, car wax). In total 29 samples of consumer products were collected in the previous study ( including food contact material, textiles, lubricants, car wax, table cloth, ski wax and more) Pressed pellets of 100-120 mg sample was homogenized, shredded for TOF for TOF In total 35 samples Samples of paper and board FCM were collected at importers or at retail shops in Norway. Relevant samples of paper and board FCM in direct contact with the food, for example muffin making cups, baking paper, snack paper, fast food packaging, pizza trays, coffee / tea cups, bags for microwave oven popcorn and similar products that have a grease and water repellent surface. Samples that have a layer of plastic in direct contact with the food were not included. Sampling was conducted in three Norwegian Food Safety Authority regions: "Greater-Oslo", "East" and "South and West". 6 cm2 na 350 consumer products purchased from 94 retail stores/vendors in April/May 2015 (paper and textile samples likely PFAS treated for water and 2 cm2 with 1 oil repellency) cm2 hole no Three different brands of wrapping papers, breakfast bags, baking papers and roasting bags samples, ob_x0002_tained from typical, commercially available food contact products in Poland sheet area 1*103 cm2 of the same thickness (~0.1 mm) was cut into small pieces na Microwave popcorn bags of three different brands from supermarkets in Spain 0.5 g samples were ground Different packaging material smade of cardboard (microwave popcorn bag, grease proof paper for French fries, cardboard box for pizza, cinema cardboard box for popcorn) and plastic (milkbottle, muffin cup, pre-cooked food wrapper, cup of coffee)were obtained randomly from local markets, restaurants and cinema 1 cm2 pieces, 0.5 g printed outside layer was removed 18 plastic empty containers were provided by two food industries of the Valencian Region (Spain) during 2016: a) six Tetrabrick were destined to contain juice (with pH<4.5) and juice with milk (with pH>4.5); b) six pouches were destined to contain milk derivates, manufactured as infant food; and c) six bags to contain musts with fruit pulp (with pH>4.5) 1 cm2 na real textile samples of different fabrics, as well as five popcorn bucket and six oil-proof hamburger wrapping paper samples, which were collected from local markets or purchased online not reported na Tefal cookware (24 cm diameter and 30mm thickness of Teflon layer which coats the inner surface of utensils), these utensils were purchased from Shedid Eng. Establishment, Cairo, Egypt. 1 g patches (tomato), 500 g patches (white beans); small square shapes (0.5-1 cm) cut from the tested utensils coated with Tefal for surface analysis 10 patches used with salt and 10 without salt for each vegetable, tomato pulp was passed through a finisher (0.5mm screen), patches white dry beans were soaked in 1 L of distilled water for 180 min. prior to cooking; tomato/ white beans were cooked in tefal utensils, samples of the respective vegetable cooked in the same container Solids (coated materials): at least 200 cm2 or 2 g, solids (non-coated): sampled according to EN ISO 8130-9 see sampling Sample materials need to ground as appropriate to ensure an efficient extraction process. Textile and paper shall be cut into pieces of maximum 1 cm2 before methanol is added. For grinding of polymers and granulates it is recommended to use EN ISO 6427 or ISO 9113. Extraction Clean up Measurement Sonification in methanol for textile, fabrics, leather and paper Concentrate the extract by a factor of 10 and use a cleanup if necessary. Active carbon cleanup and/or solid phase extraction (SPE) clean-up may be used. Transfer a known volume into a suitable LC sampling vial . If necessary dilute the original solution further and repeat the analysis LC-qMS, LC-tandemMS supramolecular solvent (SUPRAS)-based extraction, diluted 1:1 (v/v) heptanol, tetrahydrofuran, with methanol, and water mixed solvents filtered UHPSFC-(+)ESI-MS/MS In-tube solid-phase microextraction (SPME) na supercritical fluid extraction (SFE), supercritical carbon dioxide (Sc-CO2) with methanol na LC-MS HPLC/MS solid and liquid sample extraction (Liu 2012, US EPA Report, EPA/600/R-12/585) na HPLC/MS/MS Solid phase extraction, evaporation to dryness, Pressurized liquid extraction reconstitution in (PLE) with Methanol mobile phase LC/(-)ESI-MS/MS Sonification in methanol na GC/MS overheated: pans put onto a stove, heated with a 3000W stove, Gaseous emissions trapped by a precleaned glass lid, SPE; normal use: Products (consumer products, sandwich maker, waffle iron) placed in the middle of the hobbock, emission test started as the oven reached 230 C Rinsing in triplicate using methanol (normal conditions and overheated), SPE HPLC-ESI-MS FCM: Soxhlet extraction, SPE; Dust: Sonification in dichloromethane na methanol-based (0.3% methanolic ammonium hydroxide followed by rotation and centrifugation) na Dust: UPLC/(-)ESI-MS/MS, FCM: HPLC/MS/ MS, GC/PCI-MS UHPLC-MS/MS analyses were completed on a Thermo Vanquish UHPLC system (Waltham, MA, USA) coupled to a Thermo Quantis triple quadrupole mass spectrometer (operated in negative selected reaction monitoring mode) with a Phenomenex Gemini C18 column and a gradient elution using water and methanol, both with 5 mM ammonium formate Sonication with ethanol at centrifugation and 60 ^C filtering UHPLC/(-)ESI-QTOF/MS SPE with methanol and water filtered UPLC/MS/MS differ depending on the respective matrix: ion pair extraction, acidic-alkaine sequential extraction or SPE with acetone, hexane or differ depending on methyl-t-butyl ether as the respective solvent matrix PFAA: HPLC-MS/MS FTOH: GC/CI-MS Sonification in ethyl acetate for FTOHs, heated in methanol for PFASs na PIGE (total fluorine), GC-MS (FTOHs), HPLC-MS/MS (PFASs), TOP assay Sonification in methanol na GC-CSR-LVSI-MS, QTOF-MS (nontargeted analysis) methanol extraction, XPS (not extracted sample/ methanol extract) na X-ray photoelectron spectrosopy (XPS), LC(-)ESI-MS, LC-QTOF-MS Sonification in methanol (heated) WAX cartridges FTOH: UPLC-MS/MS and/or UPLC-QTOF, PFCA: UPLC-ESI(-)-MS/ MS targeted analysis: extraction in methanol na particle-induced -ray emission spectroscopy (PIGE), instrumental neutron activation analysis (InaA), combustion ion chromatography (CIC), UHPLC-MS/MS PIGE: no extraction, sonification in methanol for MS na PIGE (total fluorine), HPLC-TOF-MS (PFAS) extracted with methanol and ethyl acetate successively by shaking in an orbital shaker water added, oxidation of one aliquot by TOP assay followed by SPE (after TOP), one aliquot SPE (before TOP) TOP assay, UPLC-MS/MS (ESI) SPE (sonication for FCM) na LC/(-)ESI-MS focused ultrasonic liquid dried, reconstrituted extraction (FUSLE), ethanol with methanol UHPLC-QTOF see Zabaleta 2017 see Zabaleta 2017 LC-QqQ-MS/MS - Agilent 1260 series HPLC chromatograph coupled to an Agilent 6430 triple quadrupole (QqQ) mass spectrometer equipped with both electrospray (ESI) and atmospheric pressure chemical ionization (APCI) sources. Focused ultrasonic solid- liquid extraction (FUSLE) with methanol Envi-Carb sorbent with methanol LC-QToF-MS Ultrasonic solvent extraction (acetonitrile, acetone or 2-propanol), LLE na GC-MS/MS, HPLC-MS/MS ultrasonic liquid extraction dried, reconstrituted contact angle measurement, UHPLC-(-)ESI- (FUSLE) with ethanol with methanol MS/MS ultrasound solid-liquid extraction (FUSLE) with ethanol evaporated, reconstituted in methanol, filtered UHPLC/QTOF-MS/MS focused ultrasound solid- liquid extraction (FUSLE), Ethanol na UHPLC-(QTOF)MS/MS Sonication with water, off-line SPE na na LC-MS, Phenyl-Hexyl column applying a water/acetonitrile gradient UHPLC/(-)ESI-QTOF/MS and MS/MS (the mobile phases were adjusted to pH 2.8 with formic acid, and pH 9.7 with ammonia:) PLE with methanol ald saliva centrifugation, for saiva evaporated and reconstituted in acetonitrile LC-MS/MS ultrasonification in methanol volume reduced to 2 UPLC-MS/MS for ionic PDAS and PAP, GC/ mL, aliquot filtered MSD for FTOH LC-MS: ultrasonic extraction with matrix dependent solvents (no further information), burning for TOF and absorbtion of combustion gases in buffer LC-MS: (multi)-step- solution sample clean-up Targeted analysis with LC/MS-MS (Agilent HPLC 1290 Infinity Serie coupled with Agilent 6460A Triple Quad LC/MS-MSMS), TOF by IC Sonification in ethanol (PFCA/PFSA), 50% ethanol:water (PAP, FTOH) filtered no extraction no na na PLE with methanol na UPLC-MS/MS Particle-Induced Gamma Ray Emission (PIGE) consisted two pumps, an autosampler (set at 4C), a column oven and a system controller coupled with mass spectrometer (QTRAP 5500, AB SCIEX, All chro_x0002_matographic determinations were performed on XBridge C18 150 2.1 mm 3.5 m column (Waters, Milford, MA, USA) at 45C with the flow rate of 0.23 ml/ min. Compounds were eluted in gradient system composed of water/formic acid (99.0/1.0, phase A) and acetonitrile/formic acid (99.0/1.0, phase B). Gradient was as follows: 30% B (0.0 min), 30-80% B (0.0- 5.0 min), 80% B (5.0-20.0 min), 80-30% (20.0-21.0 min) and 30% (21.00-41.0 min) UHPLC/(-)ESI-QTOF-MS Ultrasonic probe-assisted extraction (UPAE) with methanol supernatant was filtered and evaporated to dryness LC-QqQ-MS/MS Destructive test: pieces were soaked in 3% acetic acid in water, w/v, during 2 h at 70 degrees followed by liquid-liquid extraction twice (with DCM) na dicationic ionic liquid (DIL) based easy ambient sonic- spray ionization (EASI), solvents (acetonitrile, methanol, acetone, isopropyl alcohol, dichloromethane, tetrahydrofuran, ethyl acetate, and hexane) na UHPLC-Orbitrap-HRMS EASI-MS/MS Pressurized liquid extraction (PLE) with ethanol/water (1:9 watery, 19:1 fatty) N7A LC/MS, XRD, EDX, ESEM Sonification in methanol for textile, fabrics, leather and paper Concentrate the extract by a factor of 10 and use a clean- up if necessary. Active carbon cleanup and/or solid phase extraction (SPE) clean-up may be used. Transfer a known volume into a suitable LC sampling vial . If necessary dilute the original solution further and repeat the analysis LC-qMS, LC-tandemMS Quantification method Working range (ng/mL) As Matrices Quantify the samples by using the unextracted external calibration curve. When spiking with labelled reference solutions, the determination of the concentration is independent of possible errors made during injection. Also, errors caused by sample losses during distinct steps of sample pretreatment or the adjustment of final sample extract volume as well as matrix effects in the sample are accounted for. Method is applicable for a concentration range for PFOS in the extract solution of 0,5 g/l to 50 g/l. Coated materials like paper, textile, leather, carpets, clothes and footwear, Noncoated materials, liquids internal standards N7A 32 real textile samples of different fabrics (e.g., cotton, wool, and polyester) and 6 food packaging material samples (e.g., oil-proof hamburger wrapping paper) six-point calibration environmental water, elution 0.05-5 ng mL-1 of Teflon-coated pan internal standard na solid matrices, paper, fabrics, sand internal standardisation using mass-labeled standards na carpet, commercial carpetcare liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated nonwoven medical garments, floor waxes, food-contact paper, membranes for apparel, and thread-sealant tapes isotope dilution method na internal standards na Food packaging materials carpet, commercial carpetcare liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated nonwoven medical garments, floor waxes, food-contact paper, membranes for apparel, and thread-sealant tape internal standardisation using mass-labeled internal standards na Emission from overheated pans, consumer products and FCM internal standardisation using mass-labeled internal standards na Indoor dust and packaging materials linear regression models from calibration curves built for each analyte N7A straws out of plastic, paper and plant-based external calibration was used for the semi- quantification of diPAPS and S-diPAPS na Extracts and Migrates from food contact materials internal standardisation using mass-labeled standards na food packaging materials, food internal standardisation using mass-labeled internal standards na textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes internal standards na papers (mainly food-contact material), textiles internal standardisation using mass-labeled internal standards; FTOHs derivatives were quantified using the standard curve of 10:2 FTOH derivative N7A paper and textile internal standards N7A internal standardisation using mass-labeled internal standards; FTOHs derivatives were quantified using the standard curve of 10:2 FTOH derivative na targeted analysis: internal standardisation using mass- labeled internal standards, calibration curve (naF) for CIC, Daily calibrations of PIGE signal to TF with naF, Fluoride standard for InaA calibration, N7A paper and textile paper-made FCMs french-fry bags, microwave popcorn bags PIGE: PFAS standards dissolved in methanol and dried onto filter paper (external standard), TOF: peak area as a semi- quantitative indication na paper and paperboard food wrappers for fastfood isotopic dilution method 0.1-100 ng/mL pet food and the packaging material Quantification was performed by using di- labelled 13C-PFOA as an internal standard for all PFCAs. na food contact papers, migration into food simulants internal standardisation using mass-labeled internal standards N7A Microwave packer packaging Quantification was performed with the selected reaction-monitoring (SRM) mode, internal standardisation using mass- labeled internal standards N7A paper and board (P/B) packaging materials internal standardisation using mass-labeled internal 25 ng/g and 50 standards ng/g Popcorn bag internal standardisation using mass-labeled internal standards na Paper External calibration curve, nonmass labeled standards, data independent acquisition (DIA) N7A internal standardisation using mass-labeled standards na food packaging, water and oil resistance performance food-contact packaging internal standardisation using mass-labeled standards na popcorn bags, popcorn calibration standards internal standardisation using mass-labeled standards food packaging, polytetrafluoroethylene (PTFE) sealant tape and 10 g/mL to 1000 drinking g/mL water. industrial blends and extracts 0.025-5 g mL-1 from food contact materials calibration curve food packaging materials, 0.05-10 g L-1 migrates internal standardisation using mass-labeled internal standards na Consumer products, FCM LC-MS: internal isotope- labeled standards (isotope dilution method) N7A Consumer products, Textiles, FCM Quantitation was performed using external calibration standards added several corresponding C13-labelled internal standards N7A external inorganic fluorine standard (naF) and external paper and textile standards with PFOA na paper and board FCM paper and textile na na internal standardisation using mass-labeled standards wrapping papers, breakfast bags, baking papers and roasting bags popcorn packaging internal standardisation using mass-labeled internal standards na Plastic and cardboard materials no quantification N7A juice tetrabricks, pouches and bags internal standardisation using mass-labeled internal standards N7A real textile, popcorn bucket, and oil-proof hamburger wrapping paper samples quantitative determination was evaluated via recovery experiments N7A Leaching from tefal cookware Quantify the samples by using the unextracted external calibration curve. When spiking with labelled reference solutions, the determination of the concentration is independent of possible errors made during injection. Also, errors caused by sample losses during distinct steps of sample pre- treatment or the adjustment of final sample extract volume as well as matrix effects in the sample are accounted for. Method is applicable for a concentration range for PFOS in the extract solution of 0,5 g/l to 50 g/l. Coated materials like paper, textile, leather, carpets, clothes and footwear, Noncoated materials, liquids Reported levels (ng/mL) info - validation of the method Limitations The recovery of labelled reference compound shall be in the range from 70 % to 125 % for the sample to be na considered valid. Good linearity with correlation coefficients all greater than 0.99, six replicate measurements, relative errors less than 9% PFDoA (19.85 g kg-1) and PFOA compared to HPLC-ESI-MS/ (12.49 g kg-1) (textile sample) MS na PFOA: 35.3 +/- 1.2 (Tap Water Osaka), 14.6 +/- 0.1 (Yodo River Osaka), 27.3 +/- 1.1 (Frying pan) g/mL, PFOS ND The within-day and between-day precisions (relative standard deviations) were below 3.7 and 6.0%, respectively, 81% recovery of spiked river samples for PFOA and PFOS na Extraction efficiencies (with double extractions) close to 100% for PFOA and 80% for PFOS for both paper and fabric matrices, Linear relation amounts and na response (2-1000 ng mL-1) na Individual PFCAs: ND-2600 ng g-1 product na na PFBA: 275.84 g kg-1 PFHxA: 341.21 g kg-1 PFHpA: 5.19 g kg-1 na 6:2 FTOH: ND - 331 g g(-1), 8:2 FTOG: ND - 92 g g(-1), 10:2 FTOH: ND - 24 g g(-1) Internal audit pogram (IAP) standards analzed after each calibration, Daily quality check na PFCAs: 4.75 ng/h (normal condition), 12190 ng/h (overheated at 370 C) method blank tests before and after use did not perform studies on the recovery of spiked samples PFAS: 1.3 to 69 ng g-1 (Dust), Median PFOA (FCM) = 2.40 ng g-1, Median PFOS (FCM) = 0.29 ng g-1 na na 21 PFAS were detected in the paper and other plant-based straws, with total mean PFAS concentrations (triplicate analysis) ranging from 0.043 0.004 ng/straw to 29.1 1.66 ng/straw (median = 0.554 ng/straw) na na More than 115 polyfluorinated surfactants detected, semi- quantification of diPAPS and S- diPAPS of 0.2-0.7 mg kg-1 food for popcorn migrates na na DiPAP: 0.9-36 pg/g (food), <0.001- recoveries between 72-110 4 ng/cm2 (FCM) % na PFOA: up to 2000 g/kg (ski waxes), up to 19 g/m2 (outdoor textiles), up to 15 g/m2 (baking paper) PFBA: up to 200 g/kg (leather) PFBS: up to 120 g/kg (leather) accreditations according to DIN EN ISO/IEC 17025:2005, quality control standards na na na na Total concentrations of ND-4000 ng/g (paper) and 67 to 180 000 ng/g (textile) continuing calibration verification (CCV) was analyzed at the beginning of each analysis na PFOA: 3200 nmol m-2 (0.38 mg kg-1) (carpet), PFBA: 960 nmol m- 2 (0.60 mg kg-1) (disposable bowl), 45% F from a new Duplicate injection, upholstery sample precision experiments na Average concentration of total FTOH: 2990 g kg-1 na sum PFAS concentration: 23.9 to 2220 pg/cm2 in targeted analyses, CIC: TF = 2.05-17.8 g/cm2, EOF = 0.22-0.49 g/cm2 na na Five samples with detectable total F were analyzed in duplicate for PIGE: > 200 nmol/cm2 for some PFAS to assess the samples reproducibility na Therecoveries of target PFCAs concentrations before analytes in matrix spike and after the TOP assay were 1.99 samples are shown in Table and 11.0 ng/g S3 (no access) TOP assay may not oxidize all PFAS precursors and in some cases intermediate fluorinated compounds are formed from oxidation are not measured in routine analysis, PFAS bound strongly to the matrix were not expected to be 342 extracted by this method. PFCAs: 700-2220 g kg of paper na PFOS < LOD PFOA: 22.1 and 12.9 ng dm-2 na Absence of PFCAs, PFSAs and PFPAs in all P/B samples, except in a in a Spanish microwave popcorn bag (2.1 ng/g of PFHxA) and in a Chinese microwave popcorn bag, which contained 6 PFCAs in concentrations ranging between 2.7 and 47 ng/g. Some potential precursors at low concentrations (2.1-7 ng/g of 6:2 diPAP, 4 ng/g 8:2 diPAP and 1.1 ng/g 6:2 FTUCA) have been detected in several grease proof materials na recovery values after PFBA: 250-820 ng/g, PFHxA: 174- correction with the 811 ng/g, PFPeA, PFHpA, PFOA: corresponding labeled 15 to 73 ng/g, PFHpA: 37 to 99 standard were in the 69- ng/g, PFOA: 63 to 198 ng/g 103 % and 62-98 % range na 0.0050-0.23 mg/kg Acceptable recoveries (70- 120%) and RSDs (<20%) na 1278 ppm (C4) to 38 ppm (C10) for avodaco oil na PFAA: 4-29 ng/g (PFHpA most abundant) RSDs below 11% and 15%, respectively na PFCAs at 3.50 ng/g - 750 ng/g in popcorn bags (PFHxA most abundant) The method showed good accuracy with recovery values around 100% except for thelowest chain length PFAAs, satisfactory reproducibility with RSDs under 16%, na The obtained recovery of PFOA and PFOS when spiked to microwave PFOA: 9.1 g kg-1 (microwave popcorn bag brand A and B popcorn bag brand A), 2.8 g kg-1 ranged from 79.2 to 89.6% (PTFE sealant tape) with an RSD < 10.8% na na na na highest PFOS: 92.48 ng dm-2 (fast-food container); highest PFOA: 16.91 ng dm-2 (ice cream cup); PFOS and PFOA migrated from food packaging samples through contact with saliva simulant were 4.80 and 4.55 ng dm(-2) good linearity was established for PFOS and PFOA in a range of 0.05-10 g L-1, with R2 0.9998. na Only PFOA, 8:2 FTOH and 6:2 FTOH were found in amounts at or above 1 g/m2 or 10 mg/kg or mg/L na Overall, the levels of PFCAs and PFSAs were in the low g/m2 and g/l range in the products and the levels of 6:2 FTOH were in the g/ m2 range in food packaging. The products containing highest concentration of TOF were dental floss (310 g/kg), non-stick baking ware (1.7 g/m2 ) and table cloth (0.9 g/m2 ) na na The sum of concentrations of 10 detected perfluorocarboxylic acids (PFCA) detected in 10 samples ranged from 0.0113.1 g/kg food, FTOH: 1.3 g kg1 of food Accredited analytical method (FC430) developed at DTU, the fluorotelomer alcohols (FTOH) were not yet covered by accreditation na e.g. 78-391 nmol F/cm2 (jacket), 129-597 nmol F/cm2 (jacket high F), 161-445 nmol F/cm2 (popcorn replicate measurements on bag) the same sample na Linearity, selectivity, recovery, precision, repeatability, reproducibility, LOD and limit of quantification (LOQ). linearity was observed for all analysed PFCs in the range of concentrations Breakfast bag samples (2.54-6.60 from 0.04 to 5 ng/ml. pg/cm2), roasting bag samples recovery values of 89 6.3% (0.27-0.40 pg/cm2). The analysed for PFOA and 91 7.2% for perfluorinated sulfonates were PFOS. RSD lower than 5%. not detected in any of the %ME ranged from breakfast bag samples _x0001_6% to 17.5% na PFOA: 53-198 ng g-1 RSDs below 8%, excellent recovery values, around 100% in all cases na PFBA (291ng/g), PFHxA (254.5 ng/ g) max concentrations of 6:2 FTCA (161.6 ng/g), 6:2 FTUCA (114.4 ng/g), 5:3 FTCA (24.6 ng/g) na na For the isotopic pattern a fit threshold of 90%, an allowed intensity deviation of 30%, and a mass deviation of 5 ppm were na used. na calibration curves correlation coefficients ND, PFOA: 6.5 0.62 and 5.2 of 0.9971 and 0.9993, 0.56 g/m2 triplicate analysis na PFOS: up to 52.11 ng/g (no salt), 60.33 ng/g (salt); PFOA: up to 48.44 ng/g (no salt), 54.21 ng/g (salt) na na The recovery of labelled reference compound shall be in the range from 70 % to 125 % for the sample to be na considered valid. LoD (ng/mL) Measurement subgroup - generic name na LC-MS/MS 0.2-1.6 g kg-1 (LOD), 0.6- 3.2 g kg-1 (LOQ) na SFC-MS/MS 1.5 (PFOA) and 3.2 (PFOS) pgmL-1 na LC-MS/MS 0.71 ng mL-1 (PFOA), 0.12 ng mL-1 (PFOS); LOQ: 2.36 ng mL-1 (PFOA), 0.39 ng mL-1 (PFOS) na LC-MS/MS na na LC-MS/MS 0.20-0.94- ng/g na LC-MS/MS quantification limit is the lowest calibration concentration na GC-MS 0.1 ng/h , SDL: <1.4 ng/h (PFBA), <0.8 ng/h (other PFAAs) na LC-MS/MS GC-MS: LOD = 0.03-0.22 pg, LC-MS/MS: LOD = 3.9-30 pg, 0.29-2.40 ng/g, LOD(PFPiAs) = 12.5 pg, LOD(PFPAs) = 75 pg, LOD(monoPAPs) = 50 pg, LOD(diPAPs) = 25 pg na LC-MS/MS, GC-MS na na LC-MS/MS LOD: Migrates = 15-22 g L-1; Extracts = 0.2-0.7 mg L-1 (0.2 mg L-1 PFOA, 0.008 mg L-1 PFOS) na LC-HRMS LOD = 26-660 fg, LOQ 1-3 factors higher, MLOQ(6:2 and 8:2 monoPAPs) = 16 pg/g, MLOQ(6:2/6:2 diPAPs) = 0.6 pg/g, MLOQ(8:2/8:2 diPAPs) = 6 pg/g na LC-MS/MS LOQ (PFAA) = 0.1-0.5 g/kg or 0.02-0.5 g/m2 LOD (FTOH) = 20000 g/kg na LC-MS/MS, GC-MS GC-MS: LOD = 0.37-2.4 g/ m2, LOQ = 1.2-8.1 g/m2; LC- MS: LOD = 0.016-0.18 g/m2, LOQ = 0.034-0.58 g/m2 na PIGE, GC-MS, LC-MS/MS, TOP assay 30 and 77 ng/g (paper), 19 to 34 ng/g /(textile) na GC-MS, LC-HRMS 1% for XPS, 0.063-3.7 ng g-1 (MQL) for LC-MS/MS na XPS, LC-MS, LC-HRMS MQL = 0.8-13.7 ng/L (Water/Ethanol), 10.7-52.3 ng/L (Oil) na LC-MS/MS, LC-HRMS CIC analysis: LOD(TF) = 4.11 g/g (2.91 g/dm2 for papers and 10.0 g/dm2 for paperboard), LOD(EOF) = 0.50 g/ml, 0.68 g/ml (MDL); PIGE: LOD(TF) = 0.38 g; InaA: LOD(TF) = 0.2 g of F (for m = 0,01 g LOD = 20 g/g) na PIGE, LC-MS/MS PIGE: LOD = 16 nmol/cm2, LOQ = 50 nmol/cm2, QA/QC PIGE: LOQ ~18-23 nmol/cm2 na PIGE, LC-HRMS Trace concentrations of PFBA, PFPeA, PFHxA, PFHxS (0.091-0.250 ng/g) were found, LOD/LOQ values in SI (no access) na TOP assay, LC-MS/MS 0.02-0.05 g L-1 na LC-MS/MS LOD = 1.53 (PFOA), 0.63 (PFOS) ng g-1; LOQ = 5.11 (PFOA), 2.11 (PFOS) ng g-1 na LC-HRMS SI (no access) na LC-MS/MS MDL = 0.7-3.5 ng/g na LC-HRMS 0.0013-0.046 mg/kg (LOQ) na LC-MS/MS, GC-MS LOP: 37 ppm (C10) to higher than 1238 ppm (C4) for contact angle measurement na LC-MS/MS 0.5-2.2 ng/g na LC-HRMS 0.19 (PFUna) - 0.5 ng/mL (PFOA) na LC-HRMS LOD: 25 pg/mL (PFOS, PFOA) LOD: 50 pg/mL (PFOS, PFOA) na LC-MS na na LC-HRMS na na LC-MS/MS LOD = 0.03-0.15 g/m2, only qualitative for 6:2 monoPAP, 8:2 PAP, 6:2 diPAP, 8:2 diPAP na LC-MS/MS, GC-MS TOF: About 10 pellets must be processed to sustain a LOQ of 1 mg/kg fluorine (LOQ fluoride = 0.1 mg/l for IC) na LC-MS, CIC na na 13 nmol F/cm2 (papers), 24-45 nmol F/cm2 for textiles na LC-MS/MS PIGE 0.01 to 0.05 pg/cm2 na LOD = 0.6-16 ng g(-1), LOQ = 0.3-2.3 ng/mL na LC-MS/MS LC-HRMS LOD = 0.001-0.6 ng/mL, LOQ = 0.005-2.3 ng/mL, MDL = 0.6-2.2 ng/L na LC-MS/MS na na LC-HRMS PFOA: 0.5 (LOD), 0.8 (LOQ) g/m2, PFOS: 0.4 (LOD), 0.6 (LOQ) g/m2 na EASI-MS not reported na LC-MS/MS, XRD, EDX, ESEM conc range in extract solution: 0.5 - 50 g/L LC-MS/MS Title Authors Atmospheric Chemistry of c-C(5)HF(7) and cC(5)F(8): Temperature-Dependent OH Reaction Rate Coefficients, Degradation Products, Infrared Spectra, and Global Warming Potentials. Gierczak et al. Journal J Phys Chem A The atmospheric concentrations and emissions of major halocarbons in China during 2009- 2019 Yi et al. Environ. Poll: Atmospheric HCFC-22, HFC-125, and HFC-152a at Cape Point, South Africa Kuyper et al. Environ. Sci. Technol Atmospheric Fate and Impact of Perfluorinated Butanone and Pentanone Ren et al. Environ. Sci. Technol Reconciling reported and unreported HFC emissions with atmospheric observations Lunt et al. Comparison of halocarbon measurements in an atmospheric dry whole air sample Rhoderick et al. PNAS Elementa (Wash D C). Methyl-perfluoroheptene-ethers (CH3OC7F13): measured OH radical reaction rate coefficients for several isomers and enantiomers and their atmospheric lifetimes and global warming potentials Jubb et al. Environ. Sci. Technol First Observations of the Fourth Generation Synthetic Halocarbons HFC-1234yf, HFC1234ze(E), and HCFC-1233zd(E) in the Atmosphere Vollmer et al. Environ. Sci. Technol Airborne Trifluoroacetic Acid and Its Fraction from the Degradation of HFC-134a in Beijing, China Wu et al. European Emissions of Halogenated Greenhouse Gases Inferred from Atmospheric Measurements Keller et al. Environ. Sci. Technol Environ. Sci. Technol Emissions of Halogenated Compounds in East Asia Determined from Measurements at Jeju Island, Korea Li et al. Environ. Sci. Technol Rayleigh scattering measurements of several fluorocarbon gases Zadoo et al. Large Emissions of Perfluorocarbons in East Asia Deduced from Continuous Atmospheric Measurements Saito et al. J. Environ. Monit., Environ. Sci. Technol. year Comments DOI link PFAS 2021 na 10.1021/ acs.jpca.0c10561 c-C(5)HF(7) (1H-heptafluorocyclopentene) and cC(5)F(8) (perfluorocyclopentene) 2021 na 10.1016/ j.envpol.2021.11719 CFC-11, CFC-12, HCFC-22, HCFC-141b, HCFC- 0 142b, HFC-134a 2019 na 10.1021/ acs.est.9b01612 HFC-125, HFC-152a 2019 na 10.1021/ acs.est.9b02974 Perfluoro-2-methyl-3-pentanone (PF-2M3P), Perfluoro-3-methyl-2-buytanone (PF-3M2B) 2015 na 2015 na 2014 na 10.1016/ j.scitotenv.2012.12. 056 HFC 124, HFC 142b 10.12952/ journal.elementa.00 0075 CFC-12, CFC-113, HCFC-142b, HFC-134a 10.1021/es500888v Mixtures of methyl-perfluoroheptene-ethers (CH3OC7F13, MPHEs): (E)1,1,1,2,2,4,5,5,6,6,7,7,7-tridecafluoro-3methoxy-hept-3-ene ((E)-3m-3-ene); (Z)1,1,1,2,2,4,5,5,6,6,7,7,7-tridecafluoro-3- methoxy-hept-3-ene ((Z)-3m-3-ene); (E)1,1,1,2,3,4,5,5,6,6,7,7,7-tridecafluoro-4RSmethoxy-hept-2-ene; ((E)-4m-2-ene), (E)1,1,1,2,2,3,5,5,6,6,7,7,7-tridecafluoro-4methoxy-hept-3-ene ((E)-4m-3-ene), ( Z ) 1,1,1,2,2,3,5,5,6,6,7,7,7-tridecafluoro-4methoxy-hept-3-ene; ((Z)-4m-3-ene), (E)1,1,1,2,2,3,4,5,6,6,7,7,7-tridecafluoro- 5RSmethoxy-hept-3-ene ((E)-5m-3-ene) isomers 2014 na 10.1021/es505123x HFC-1234yf (2,3,3,3-tetrafluoroprop-1-ene, CF3CF=CH2), and HFC-1234ze(E) (E-1,3,3,3- tetrafluoroprop-1-ene trans-CF3CH=CHF), and the hydrochlorofluorocarbon HCFC-1233zd(E) (E1-chloro-3,3,3-trifluoroprop-1-ene transCF3CH=CHCl) 2014 na 10.1021/es4050264 Trifluoroacetic acid (TFA) 2012 na 10.1021/es202453j HCFC-142b (CH3CF2Cl) 2011 na CFC-12, CFC-113, CFC-114; HCFC142b, HFC134a, HFC-125, HFC-143a, HFC-365mfc, H-1211, 10.1021/es104124k CF4, C2F6, C3F8 2011 na 2010 na 10.1039/ c1em10667h hexafluoropropene (HFC-216), 1,1,1,2,3,3,3,heptafluoropropane (HFC-227ea), and octafluorocyclobutane (C-318) PFC-116 (C2F6), PFC-218 (C3F8), and PFC-318 (c10.1021/es1001488 C4F8) CAS (if available in publication) Sampling na na sample amount used 5.32 10^15 and 4.23 10^16 molecule/cm-3 From July 2009 to July 2019, we sampled in January, April, July and October, representing winter, spring, summer and autumn, respectively (samples were not collected in July and October 2015 because of equipment failure). Air samples were collected continuously for 4-7 days in each month and at 14:00 (China standard time) simultaneously at each site every day. And they were collected quarterly using evacuated electro- polished stainless-steel canisters (3.2L Silonite SummaR Style Canisters, Entech Instruments Inc.) cleaned by a canister cleaner (Entech 3100A, Instruments Inc., USA) with high purity nitrogen in advance at Peking University. In urban sites, samples were collected at a height of 2 m on the rooftops of 8-18-story buildings (20-50m above ground). And in suburban sites, samples were collected at a height of 2 m above the ground to ensure favorable diffusion of the air mass (Barletta et al., 2006). Moreover, sampling was delayed if it was rainy, snowy or hazy. During sampling, the canister valve was opened slightly over 1-2 min to ensure the surrounding air was evenly mixed. na During this period, 1902 samples were collected. 400 ml na na na na na na One litre of ambient air is passed through the adsorbents at a trapping temperature of -30 C, and then desorbed by heating the trap at 60 C/s up to 300 C, and held at One litre of na this temperature for 2 min. ambient na na na na na Manometrically prepared mixture (0.0023 mixing ratio in He) Routine ambient measurements at the two sites are characterized by a pair of hourly ambient air sample measurements from cryogenically preconcentrated 2 L samples, bracketed by na calibration standard measurements. 2 l For each gas-phase sample, the two denuders were extracted with three consecutive additions of double-distilled water (10, 10, and 5 mL) by transferring each addition from the first denuder to the second, with shaking in each denuder, and na a combined extract (25 mL) was obtained. na na na na Ambient concentrations of halogenated na compounds have been analyzed every two hour na na na na na na na Pre- treatment na Extraction Clean up SPE, PLE na Air samples would be concentrated in a cryogenic Briefly, 400 ml air preconcentration system sample was extracted (Entech 7100A, Entech into multistage traps Instruments Inc., USA) before to remove H2O, CO2 being introduced into the GC and other interfering for analysis. gases, na Samples and standards were autonomously preconcentrated on a triple- bed microtrap (3 mg Carbotrap B, 5 mg Carboxen 1003, and 4 mg Carboxen 1000) at -50 C in the ADS. na na na na na on-line sample enrichment using adsorbent material na na na na na The MPHE samples were purified by repeated freeze-pump-thaw cycles prior to the preparation of dilute mixtures in He-bath gas. na na na na na For each particle sample, the 47 mm ringed filters were weighed before and after sampling to determine particle mass (PM2.5) Particles were then entirely extracted using two consecutive additions of double- distilled water (each 10 mL) and subjected to ultrasonication for 30 min, using an additional 5 mL of water for rinsing. The combined particle extract (25 mL) was centrifuged prior to analysis. A field blank was analyzed along with every set of samples. na In situ measurements na na "Medusa" cryogenic preconcentration system na na na na na na na na Measurement FTIR (Infrared absorption processed via Fourier Transformation) Mass spectrometry was used for analysis. It should be noted that during 2009-2019, three GC-MS instruments were used for analysis, which were Varian Saturn 2100 GC-MS, Varian Co. USA (2009.7-2015.4) described by Fang et al. (2012b), Medusa-6890/5975B GC-MS, Agilent Co. USA (2016.1-2017.4) described by Zhang et al. (2017), and Trace 1300 ISQ GC-MS, Thermo Fisher Co. USA (2017.7-2019.7). Agilent gas chromatograph-mass spectrometer (GC-MS, 6890/5973N) with a custom-built adsorption/desorption system (ADS) The UV-vis absorption spectra of PF-2M3P, PF-3M2B were measured using a spectrophotometer equipped with a 1200 grooves mm-1 grating and a charge-coupled device (CCD) camera. The collimated output of a 30 W deuterium lamp passed through a 100 cm long and 2.5 cm diameter Pyrex absorption cell equipped with quartz windows and focused onto the entrance slit of the spectrometer. Measurements were made over the wavelength region 220-400 nm by recording typically three overlapping regions of about 15 nm. Typically, each measurement consisted of 8-13 scans of diode array. The wavelength scale was calibrated using the emission lines from a lowpressure Hg pen ray lamps (253.7, 313.2, and 365 nm). gas chromatography-mass spectrometry (GC-MS) preceded by on-line sample enrichment using adsorbent material. A GC-MS Agilent 6850- 5975 has been equipped with auto-sampling/ pre-concentration device (Markes International, UNITY2-Air Server2) to enrich the halocarbons on a focussing trap filled with four different adsorbing materials: Carbograph 2TD, Carbograph 1TD, Carboxen 1000 and Carbosieve SIII, and kept chilled at sub-ambient temperature by a three stage Peltier cell. One litre of ambient air is passed through the adsorbents at a trapping temperature of -30 C, and then desorbed by heating the trap at 60 C/s up to 300 C, and held at this temperature for 2 min. The separation is performed on a J&W GS-GasPro capillary column, 30 m0.32 mm I.D., at 1.6 ml min-1, at constant flow; the temperature ramp is 10 min at 49 C, then 10 C min-1, up to 250 C for a total run time of about 40 min. NIST: GC-ECD, GC-MS, GC-FID NOAA: GC-ECD, GC-MSD KRISS: GC-ECD, GC-MSD SIO: GC-ECD (GC-MD)b, GC-MSD (Medusa) EMPA: Medusa-GC-MS technology (Empa-medusa or Medusa-20) FTIR (Infrared absorption processed via Fourier Transformation) 296 K over the range 500 to 4000 cm-1 The samples were analyzed using gas chromatography - mass spectrometry (GCMS) with "Medusa-GCMS" type instruments. TFA and the internal standard [perfluoropropionic acid (PFPA)] were derivatized to the respective acid anilide in the presence of 2,4-DFAn and DCC. Samples were cleaned and reduced to 1 mL for analysis using GC-MS (QP-2010 SE, Shimadzu, Kyoto, Japan) with ions of 225 and 275 amu for TFA and PFPA, respectively. GC separation was performed using a DB-5 ms column (30 m 0.32 mm 0.25 m) with helium as a carrier gas. The initial oven temperature was 50 C for 2 min, after which it was increased at a rate of 30 C/min to a maximum temperature of 215 C and then maintained at that temperature for another 10 min. The injector, transfer line, ion source, and detector temperatures were maintained at 200, 250, 200, and 250 C, respectively. Using LC-MS/MS, extracts were directly injected into LC (UFLC XR, Shimadzu, Kyoto, Japan) interfaced to a 4000Q TRAP (MDS Sciex, Concord,Ontario, Canada) operated in the negative electrospray ionization mode. LC separation was performed using a Rspak JJ-50 2D column (2.0 mm 150 mm 5 m, Shodex, Showa Denko K.K., Kawasaki, Japan) at a flow rate of 200 L/min via an isocratic elution. For mobile phase A, we used 20% 50 mM ammonium acetate in water, and for mobile phase B, we used 80% methanol and 20% water. The MS/MS transition used to quantify TFA was m/z 112.9/68.9. Gas chromatograph/mass spectrometer (Agilent 6890/5973) coupled to an adsorption desorption system (ADS). Air samples were taken every 2 h at a height of 9.4 m above ground Gas chromatograph and mass selective detector (GC-MSD)13 as part of the Advanced Global Atmospheric Gases Experiment (AGAGE) network. A Radiance Research M903 Integrating Nephelometer was equipped with a 530 nm (_x0003_40 nm FWHM) band-pass filter to constrain measurement wavelength. The nephelometer was modified in the laboratory to monitor the photomultiplier output pulse on a Tektronix TDS 1012B Two Channel Digital Storage Oscilloscope. Recorded measurements were peak-to-peak voltage signal of the pulsed light source. Measurements were the result of averaging 64 pulses. The peak-to-peak signal was found to scale linearly with gases of known scattering coefficient (air, CO2, R-134a) as illustrated in Fig. 1B. A IST traceable digital hygrometer (Fisher Scientific) was used to monitor the Celsius temperature and relative humidity at the outlet of the measurement cell to one decimal digit of precision. The internal pressure sensor of the nephelometer was used to monitor cell pressure to within 1 mbar. Conditions t measurement were generallyz 915-930 mbar, 21 _x0005_C, and 0.1% RH, however care was taken to always log the exact temperature and pressure data to account for differences in gas density between trials. HEPA filters were placed prior to the nephelometer purge inlet and at the outlet of the flow ystem to prevent particle contamination ambient air is analyzed every hour with a fully automated preconcentration/gas chromatography/ mass spectrometry (GC/MS) system Quantification method Working range (ng/mL) As The absorption spectra were quantified by a linear leastsquares fit to Beer's law na A multipoint external calibration method was used to analyze target compounds. TO-14A (Spectra Gases, USA) and the standard gas provided by the National Institute of Metrology of China (NIMC) were applied for the calibration of CFCs, HCFCs and HFCs. Before analyzing the samples, calibration gas was diluted to 9 concentration levels with ultrapure nitrogen. The coefficient of determinations (R2) of the calibration curves were over 0.990 for each target compound. na Calibrated mole fractions were assigned to short-term working standards from an external long-term working standard tank which was calibrated using the Advanced Global Atmospheric Gases Experiment (AGAGE) Medusa GC-MS at Mace Head. na Lambert Beer concentration ranges [PF-2M3P] = (0.29-2.7) 1017, [PF-3M2B] = (0.27-3.0) 1017 For maximum sensitivity in routine field monitoring, the MS detector is operating in selective ion mode (SIM); since many compounds have similar electron impact (EI) fragmentation paths, identification and quantification are based on two mass-overcharge ratios (m/z) per compound (target ion and at least one qualifier), in order to improve the diagnostic for determining chromatographic co-elution The targeted trace gas species exhibit awide range of volatilities and atmospheric abundances; typical concentrations are in the ppt (10-12) range NIST: GLS, 2nd order polynomial, linear, or bracketing NOAA:2nd order polynomial or linear KRISS: One point calibration SIO: Primary calibration in sensitivity space EMPA:Bracketing na The measured spectra obeyed Beer-Lambert's law with a precision of 1% (2). na na na The MS/MS transition used to quantify TFA was m/z 112.9/68.9. na na na na na na na na na Matrices info - validation of the Reported levels (ng/mL) method Limitations 0.18-2.21 x 10^16 Ambient air molecule / cm-3) na na HCFC-22 increased from 627 405 pptv in 2009 to 743 355 pptv in 2019 with a rate of 11.1 pptv yr-1 HFC-134a had a significant increase from 76 30pptv to 186 72 pptv (2009-2019), with a fast growth rate of 10.6 pptv yr- 1, almost twofold of 5.6 0.2 pptv yr- 1 (2012-2016) globally Ambient air reported by na na HFC-125: 22.47 1.78 ppt HFC-152a: 6.44 5.32 ppt Ambient air na na Ambient air na na na Ambient air ppt na na Dried whole air sample na na na (0.455-10.2) 1015 molecules Ambient air cm-3 na na Ambient air ppt na na Ambient air Ambient air mean concentration of TFA was 1580 558 pg/m3 (mean standard deviation) na na 1010 -1820 To detect and correct for drift in detector sensitivity, every 11th sample was taken from a real-air calibration standard. na Ambient air 0,1-134,6 kt/a The compounds measured here are on calibration scales developed at the Scripps Institution of Oceanography (SIO)14 with the exception of HFC-125 and CH2Cl2 which are on the UB-98 scale (University of Bristol) and HFC-365mfc which is on the Empa2003 scale (Swiss Federal Laboratories for Materials Science and Technology). na na na na na Ambient air ppt na na LoD (ng/mL) subgroup Measurement - generic name na F-Gases FTIR The method detection limit analyzing by Trace 1300 ISQ GC-MS was 2.3- 38.8 pptv and the measurement precision was 2.2-3.4% GC-MS na na GC-MS na na UV-VIS spectro LOD: 0,13-0,52 ppt na na na GC-MS GC-MS na F-Gases FTIR na na GC-MS na na na na GC-MS GC-MS na na GC-MS na na na na sensor GC-MS Title AIRBORNE AEROSOLS IN APPLICATION OF POLYFLUORO POLYMER-BASED SKI WAXES CEN/TS 15968:2010 - Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LCqMS or LC-tandem/MS Perfluoroalkyl and polyfluoroalkyl substances in consumer products Analysis of per- and polyfluorinated substances in articles Analysis of PFASs and TOF in products Screening of Semifluorinated n-Alkanes by Gas Chromatography coupled to Dielectric Barrier Discharge Ionization-Mass Spectrometry (GC/DBDI-MS) Levels of per- and polyfluoroalkyl substances (PFAS) in ski wax products on the market in 20 PFAS i kemiska produkter och varor Ett tillsynsprojekt med fokus p POPs-frordningens begrnsningar av PFOA och PFOS (PFAS in chemical products and articles A regulatory project focusing on the POPs Regulation restrictions on PFOA and PFOS) Authors Liesivuori et al. Journal year Annals of Occupational Hygiene 1994 Vol. 38 I 1994 Standard Kotthoff et al. na Environ Sci Pollut Res Int 2010 2015 Blom et al. Borg et al. Nordic Council of Ministers 2015 Nordic Council of Ministers 2017 Hagenhoff et al. Rapid Communications in Mass Spectrometry 2 2018 Fang et al. KEMI Environmental Science: Processes & Impacts 2019 na 2021 comments na DOI link 10.1093/annhyg/38.6.931 Also used for other matrices, sample treatmant different na na 10.1007/s11356-015-4202-7 na http://dx.doi.org/10.6027/na2015-911 na http://dx.doi.org/10.6027/ na 10.1002/rcm.8139 na Several matrices tested: Textiles, Ski wax, and other consumer products 10.1039/d0em00357c na name PFOS, PFOSA, N-Me-FOSA, N-Et-FOSA, N-Me-FOSE alcohol, N-Et-FOSE alcohol, PFOS salt PFBA, PFPA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUna, PFDoA, PFTrA, PFTeA, PFBS, PFHxS, PFHpS, PFOS, PFDS, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, PFOSA PFCAs (PFBA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA), PFASs (PFBS, PFHxS, PFOS), PAPs (6:2 diPAP, 6:2 monoPAP, 8:2 diPAP, 8:2 mono-PAP), FTOH (4:2, 6:2, 8:2), FTS (4:2, 6:2) TOF, targeted analysis of PFCAs (PFBA, PFHxA, PFOA, PFna, PFDA), PFSAs (PFBS, PFHxS, PFOS), FTOHs (4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH), FTAs (6:2 FTA, 8:2 FTA, 10:2 FTA), FOSAs (MeFOSA, EtFOSA), FOSEs (MeFOSE, EtFOSE) 1-(perfluorobutyl)pentane (F4H5), 1-(perfluorobutyl)hexane (F4H6), 1-(perfluoro_x0002_butyl)octane (F4H8), and 1(perfluorohexyl)octane (F6H8), 1-(Perfluorohexyl)tetradecane (F6H14), and 1-(perfluorooctyl)hexadecane (F8H16), 1-(Perfluorohexyl)oct-1-ene (F6H8ene) Perfluorobutanoic acid (PFBA, C4) Perfluoropetanoic acid (PFPeA, C5) Perfluorohexanoic acid (PFHxA, C6) Perfluoroheptanoic acid (PFHpA, C7) Perfluorooctanoic acid (PFOA, C8) Perfluorononanoic acid (PFna, C9) Perfluorodecanoic acid (PFDA, C10) Perfluoroundecanoic acid (PFUnDA, C11) Perfluorododecanoic acid (PFDoDA, C12) Perfluorotridecanoic acid (PFTrDA, C13) Perfluorotetradecanoic acid (PFTeDA, C14) Perfluoropentadecanoic acid (PFPeDA, C15) Perfluorohexadecanoic acid (PFHxDA, C16) Perfluoroheptadecanoic acid (PFHpDA, C17) Perfluorooctadecanoic acid (PFODA, C18) Perfluorononadecanoic acid (C19) Perfluoroeicosanoic acid (C20) Perfluoroheneicosanoic acid (C21) Perfluorodocosanoic acid (C22) Perfluorotetracosanoic acid (C23) Perfluorotricosanoic acid (C24) Perfluoropentacosanoic acid (C25) PFAS Tests according to CEN/TS 15968:2010 EOF not further described CAS (if available in source) na 1763-23-1 (PFOS) 754-91-6 (PFOSA) 24448-09-7 (N-Me-FOSE alcohol) 1691-99-2 (N-Et-FOSE alcohol) na 375-22-4 (PFBA), 307-24-4 (PFHxA), 375-85-9 (PFHpA), 335-67-1 (PFOA), 375-95-1 (PFna), 33576-2 (PFDA), 4234-23-5 (PFUnDA), 307-55-1 (PFDoDA), 72629-94-8 (PFTrDA), 376-06-7 (PFTeDA), 29420-49-3 (PFBS salt), 3871-99-6 (PFHxS salt), 1763-23-1 (PFOS salt), 2043-47-2 (4:2 FTOH), 647-42-7 (6:2 FTOH), 678-39-7 (8:2 FTOH), 57677-95-9 (6:2 diPAP), 57678-01-0 (6:2 monoPAP), 678-41-1 (8:2 diPAP), 57678-03-2 (8:2 mono-PAP), 757124-72-4 (4:2 FTS), 2942049-3 (6:2 FTS) 375-22-4 (PFBA), 2942049-3 (PFBS salt), 307-24-4 (PFHxA), 3871-99-6 (PFHxS salt), 2043-47-2 (4:2 FTOH), 757124-72-4 (4:2 FTS), 335-67-1 (PFOA), 1763-23-1 (PFOS salt), 647-42-7 (6:2 FTOH), 29420-49-3 (6:2 FTS), 31506-32-8 (MeFOSA), 4151-50-2 (EtFOSA), 2448-09-7 (MeFOSE), 1691-99-2 (EtFOSE), 37595-1 (PFna), 335-76-2 (PFDA), 678-39-7 (8:2 FTOH) na na Tests according to CEN/TS 15968:2010 Sampling sample amount used aerosol sampling on mixed cellulose ester membrane filters. ski-wax fume sampling was done with Tenax-polymer tubes na Liquids: method which will provide a representative sample of the liquid to be tested. see sampling 115 samples of consumer products including textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes. The individual samples analysed were bought from local retailers or collected by co-workers of the institute or local clubs (e.g. ski waxes from local skiing club). The sampled products span all quality levels from entry level to cutting edge products. The selection of the samples occurred randomly. na In total 29 different samples were analysed. The sampling was concentrated on a few but wide variety of household products, such as cleaning products and polishes for indoor use and for cars and sprays to waterproof shoes or clothes, food contact paper and baking forms included some products less commonly analysed, such as ski wax, dental floss and tablecloths. The samples were purchased in the vicinity of Oslo in supermarket chains that are found all over Norway. depending on the article: 0.05 mL, 71.5-100 cm^2 or 0.02-0.16 g In total 17 products were randomly selected from shelves in a number of Swedish retail stores and supermarkets for analysis (Cupcake forms, microwave popcorn bag, rinse aid, waterproofing shoe treatment, waterproofing textile treatment, shoe wax, floor polish, furniture polish, car wax). In total 29 samples of consumer products were collected in the previous study (including food contact material, textiles, lubricants, car wax, table cloth, ski wax and more) Pressed pellets of 100-120 mg for TOF ski wax dissolved in cyclohexane na 11 separate commercially available and best-selling ski wax products were purchased from one of Norway's largest sports stores in the summer of 2019. The ski wax products comprised; 3 wax blocks, 1 liquid wax and 7 powders. 10 mg Tests according to CEN/TS 15968:2010 Tests according to CEN/TS 15968:2010 Pre- treatment na Dilution for AFFF: Pre-dilute the sample in separate steps with purified water or methanol (1:10 v/v, 1:100 v/v, 1:1 000 v/v) and mix sufficiently (e.g. 500 l sample into 4 500 l diluent). Ensure that there is no phase-separation in the sample. If necessary centrifuge the sample to precipitate non soluble particles. Dilute the pre-diluted sample 1:10 with water or methanol and an appropriate volume of internal standard solution (e.g. 100 l diluted sample, 100 l reference solution, 800 l water or methanol) to have in every dilution (1:10 v/v, 1:100 v/v, 1:1 000 v/v) the same concentration of the internal standard. Transfer an aliquot to a LC vial and analyse the sample. If high PFOS concentrations are expected, begin with the highest dilution (1:10 000 v/v) to avoid a carry over. na vortexing in methanol sample was homogenized, shredded for TOF na na Tests according to CEN/TS 15968:2010 Extraction na Clean up na no extraction na differ depending on the respective matrix: ion pair extraction, differ depending acidic-alkaine sequential extraction or SPE with acetone, hexane on the respective or methyl-t-butyl ether as solvent matrix ultrasonification in methanol volume reduced to 2 mL, aliquot filtered LC-MS: ultrasonic extraction with matrix dependent solvents (no LC-MS: (multi)- further information), burning for TOF and absorbtion of step-sample clean- combustion gases in buffer solution up na na 10 mg (accurately weighed) of ski wax spiked with 0.5 ng of internal standards was extracted with 5 mL methanol. The wax/ methanol mixture was vortexed and extracted in an ultrasonic bath for 20 min and then stored at room temperature overnight. The mixture was placed in an ultrasonic bath for 20 min again the next day and then centrifuged (3000 rpm, 10 min) to facilitate sedimentation of the extracted solids. A 4 mL aliquot of the supernatant was transferred to a 13 mL polypropylene tube. The extraction of ski wax was repeated and the supernatant solutions combined. Following extraction, the 8 mL of supernatant was evaporated to approximately 200 L and 25 L recovery standard (M8PFOS and M8PFOA, both 20 pg L-1) and 200 L 4 mM NH4OAc in water were added. The extracts were then transferred to a polypropylene (PP) centrifuge tube with a nylon membrane filter and centrifuged at 13000 rpm for 5 min. The filtered extract was transferred to an autosampler vial and stored at 4 C until analysis. na Tests according to CEN/TS 15968:2010 Tests according to CEN/TS 15968:2010 Measurement high resolution gas chromatography fluoride measurements: S176 (NIOSH, 1977) and 7903 (NIOSH, 1984) LC-qMS, LC-tandemMS PFAA: HPLC-MS/MS FTOH: GC/CI-MS UPLC-MS/MS for ionic PFAS and PAP, GC/MSD for FTOH Targeted analysis with LC/MS-MS (Agilent HPLC 1290 Infinity Serie coupled with Agilent 6460A Triple Quad LC/MS-MSMS), TOF by IC hyphenation of GC with DBDI-MS (headspace and GC) PFAS were quantified using an ultra-performance liquid chromatography-tandem mass spectrometer (UPLC-MS/MS) instrument (Waters, ACQUITY-UPLC/XEVO-TQS) fitted with a BEH C18 column (1.7 m particles, 2.1 50 mm; waters). The mass spectrometer (MS) was operated in negative electrospray ionization multiple reaction monitoring (MRM) mode with the following MS parameters: capillary voltage 1100 V; nebulizer gas flow at 7 bars; desolvation gas flow at 600 L h-1; cone gas flow at 150 L h-1. The desolvation temperature was 350 C. The m/z cone voltages and collision energies used for each PFAS are listed in Table S2. Tests according to CEN/TS 15968:2010 Quantification method na Quantify the samples by using the unextracted external calibration curve. When spiking with labelled reference solutions, the determination of the concentration is independent of possible errors made during injection. Also, errors caused by sample losses during distinct steps of sample pre-treatment or the adjustment of final sample extract volume as well as matrix effects in the sample are accounted for. internal standardisation using mass-labeled internal standards internal standardisation using mass-labeled internal standards LC-MS: internal isotope-labeled standards (isotope dilution method) identification Quantification of all target analytes was performed using an internal standard calibration curve with nine points (0.008-150 ng mL-1, R2 > 0.99). Stable isotope mass labelled internal standards were available for C4-C6 and C8-C12 PFCAs, as well as for PFHxS and PFOS. C7 and C13-25 PFCAs, PFBS and PFDS were quantified using 13C2-perfluorohexanoic acid (PFHxA), 13C2-perfluorododecanoic acid (PFDoDA), 18O2-perfluorohexane sulfonate acid (18O2-PFHxS) and 13C4perfluorooctane sulfonate acid (13C4-PFOS) as internal standards, respectively. Reference standards for native C15, C17 and C19-25 PFCAs were not available. Therefore, for quantification of C15, C17 and C19-25 PFCAs the relative response factors (relative to 13C2-PFDoDA) were calculated from the calibration curves of C14, C16 and C18 PFCAs, respectively. All reported concentrations for C15, C17 and C19-25 PFCAs should thus be considered as semi-quantitative estimates due to the lack of authentic native standards for these compounds. The method detection limit (MDL) was defined as the lowest calibration point concentration resulting in a signal-to-noise ratio of three, if the specific PFAS were not detected in the blanks. For the analytes which were detected in the blanks, MDLs were defined as the mean blank concentration plus three times the standard deviation of the blank. Tests according to CEN/TS 15968:2010 LoD (ng/mL) subgroup The detection limit for fluoride in the air samples was 9 g/m3 na Measurement - generic name HR-GCMS na na LOQ (PFAA) = 0.1-0.5 g/ kg or 0.02-0.5 g/m2 LOD (FTOH) = 20000 g/ kg na LC-MS/MS LC-MS/MS, GC-MS LOD = 0.03-0.15 g/m2, only qualitative for 6:2 monoPAP, 8:2 PAP, 6:2 diPAP, 8:2 diPAP na TOF: About 10 pellets must be processed to sustain a LOQ of 1 mg/kg fluorine (LOQ fluoride = 0.1 mg/l for IC) na LC-MS/MS, GC-MS LC-MS/MS , CIC single digit pg range injected on na GC-MS 0.1-2.5 ng g-1 na LC-MS/MS Tests according to CEN/TS 15968:2010 Tests according to CEN/TS 15968:2010 usable for solid items Title Authors Journal year Comments DOI link Concentrations and trends of perfluorinated chemicals in potential indoor sources from 2007 through 2011 in the US Liu et al. Chemosp here 2014 na 10.1016/ j.chemospher e.2013.10.001 Are imported consumer products an important diffuse source of PFASs to the Norwegian environment? Vestergren et al. Environm ental Pollution 2015 na Suspect screening of 200 hazardous substances in plastic toys using ultra-high- performance liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry Meng et al. J Chromato 2020 na Perfluoroalkyl and polyfluoroalkyl substances (PFASs) in consumer productsin Norway - A pilot study Herzke et el. Chemosp here 2012 na 10.1016/ j.envpol.2014. 12.034 10.1016/ j.chroma.2019 .460830 10.1016/ j.chemospher e.2012.03.035 Perfluoroalkyl and polyfluoroalkyl substances in consumer products Kotthoff et al. Survey of perfluorinated compounds in consumer products by liquid chromatography-tandem mass spectrometry Lee et al. Environ Sci Energy & Environm ent 2020 Vol. 31 Issue 4 Pages 713-729 2015 na 2019 na 10.1007/s1135 10.1177/0958 305x1988237 6 CEN/TS 15968:2010 Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LCqMS or LC-tandem/MS Also used for other matrices, sample 2010 treatmant different Screening for perfluoroalkyl acids in consumer products, building Chemosp materials and wastes Becanova et al. here 2016 na 10.1016/ j.chemospher e.2016.08.112 0045-6535/ Screening of textile finishing agents available on the Chinese market: An important source of per- and polyfluoroalkyl substances to the environment Surfactants and other liquid matrices Mumtaz et al. Frontiers of Environm ental Science & Engineeri ng 2019 Vol. 13 Issue 5 2019 na 10.1007/ s11783-0191145-0 Removal of Per- and Polyfluoroalkyl Substances (PFASs) in Aqueous FilmForming Foam (AFFF) Using Ion-Exchange and Nonionic Resins Fang et al. Environ Sci Technol Focus on removal of 2021 PFAS 10.1021/ acs.est.1c0076 9 Reconstructing the Composition of Per- and Polyfluoroalkyl Substances in Contemporary Aqueous FilmForming Foams Ruyle et al. Environ Sci Technol Lett 2021 EPA method 10.1021/ acs.estlett.0c0 0798 Determination of total oxidizable precursors in foam surfactants and foam contaminated water based on UV-activated persulfate oxidation Fan et al. Sci Total Environ 2021 na Assessment of PFAS fate, transport, and treatment inhibition associated with a simulated AFFF release within a WASTEWATER treatment plant Chemosp here 262: Gonzalez et al. 127900. 2021 na 10.1016/ j.scitotenv.202 0.142943 10.1016/ j.chemospher e.2020.12790 0 PFAS CAS (if available in publication 9 PFCAs (C4 to C12), 5 PFASs (C4, C6, C7, C8, C10) na C4-C14 PFCAs, C4, C6 ,C8 ,C10 PFSAs, 4:2, 6:2, 8:2 and 10:2 FTOHs, N-ethyl perfluorooctanesulfonamidoethanol (EtFOSE), N- Methyl perfluorooctane sulfona-midoethanol (MeFOSE), N-Ethyl perfluorooctane sulfonamide(EtFOSA) and N-Methyl perfluorooctane sPuelrffolunoarmoipdeen(tManeoFiOc SaAci)d na Perfluorobutanesulfonic acid Perfluorohexanoic acid Perfluoroheptanoic acid Perfluorooctanoic acid Perfluorononanoic acid Perfluorooctanesulfonic acid Perfluorodecanoic acid Perfluoroundecanoic acid Perfluorododecanoic acid Pentacosafluorotridecanoic acid Perfluoromyristic acid Perfluoropalmitic acid Perfluorooctadecanoic acid na PFAS (i.e. C4-C14 PFCAs, C4,C6,C8,C10 PFSAs, 6:2 and 8:2 fluorotelomersulfonates (FTSs), PFOSA, 4:2, 6:2, 8:2, 10:2 FTOH na PFBA, PFPA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFTrA, PFTeA, PFBS, PFHxS, PFHpS, PFOS, PFDS, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, PFOSA na PFHXA, PFHpA, PFOA, PFNA, PFDA, PFBS, PFHxS, PFOS, PFOSA, N-MeFOSA, N-EtFOSO 307-24-4, 375-85-9, 335-67-1, 375-95-1, 335-76-2, 375-73-5, 355-46-4, 1763-23-1, 754-91-6, 31506-32-8, 4151-50-2 PFOS, PFOSA, N-Me-FOSA, N-Et-FOSA, N-Me-FOSE alcohol, N-Et-FOSE alcohol, PFOS salt 1763-23-1 (PFOS) 754-91-6 (PFOSA) 24448-09-7 (N-Me-FOSE alcohol) 1691-99-2 (N-Et-FOSE alcohol) PFPA, PFHxA, PFHpA, PFOA, PFNa, PFDA, PFUnDA, PFDoDa, PFTrDA, PFTeDA, PFBS, PFHxS, PFHpS, PFOS and PFDS na Targeted and non-targeted PFAS na 48 targeted PFAS (12 found: PFCAs (n = 3-7), PFSAs (n = 3-8), Cl-PFSA (n = 8)) and 63 semi-quantificated PFAS including AmPr-FASA (n = 2-6), AmPr-FASA-PrA (n = 2- 6), CEtAmPr-FASA-PrA (n = 2-6), Cl-PFSA (n = 4-6), CMeAmPr-FASA (n =4-6), CMeAmPr-FAS-PrA (n = 3-6), F5S-PFAS (n = 6), FASA (n = 4,6), PFCAs (n = 5), PFSAs (n = 3,4,6,7,8,10), UPFAS (n = 7,8), KPFAS (n = 5-8), MeEtCMeAmPr-FAAd (n = 4), MeFASAA (n = 5, 6), OAmPr-FASA (n = 5,6), O-PFAS (n = 5,6), PFASi (n = 4-6), PFCPeCA (n = 6), TAmPr-FASA (n = 3-6), TAmPr- FASAPrA (n = 3-6), UPFSA (n = 6-8) and 63 semi- quantificated PFAS na 27 targeted PFAS including PFCAs (PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA), PFSAs (PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS), FTSAs (4:2, 6:2, 8:2, 10:2), FBSA, FHxSA, FOSA, non-targeted PFAS, TF (total fluorine), EOF (extractable orgonofluorine), IF (inorganic fluorine), TOP (total oxidizable precuror) identified PFAS: 1513864-10-2 (6:2 FTSAS-sulfoxide), 88992-45-4 (6:2 FTSHA), 88992-47-6 (6:2 FTSAS), 64972-10-7 (6:2 FTThPrAm), 27619-97-2 (6:2 FTSA), 34455-29-3 (6:2 FTSA-PrB), 80475-32-7 (6:2 FTNO), 76201-56-4 (EtOH-Am-PrPFHxSAPrS), 151386418-9 (6:2 FTSOOHPrTAm) Targeted PFCAs before/after TOP asssay na na na Sampling sample amount used Pre- treatment 95 samples from 35 consumer products including carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non- woven medical garments, floor waxes, food-contact paper, membranes for apparel, and thread-sealant tapes. They were purchased from retail outlets in the United States between March 2007 and September 2011. 5 x 5 cm solid products were cut into smaller subsections. Liquid products were subdivided into at least three 30-mL polypropylene vials 45 furniture textile, carpet, clothing and food contactmaterial samples were purchased from three major retail stores inTroms and Trondheim during the period November2012eFebruary 201 10 x 10 cm samples were cut into small pieces and spiked with masslabeled internal standard pulverized after freezing 0,2 g 30 products in 6 different product groups: waterproofing agents, paint, coated fabrics, non-stick ware, electronics and fire fighting agents. They were purchased from retailers in Norway and Sweden. 1 g dissolvation- precipitation of polymers Liquid and solid samples were homogenized 115 samples of consumer products including textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes. The individual samples analysed were bought from local retailers or collected by co-workers of the institute or local clubs (e.g. ski waxes from local skiing club). The sampled products span all quality levels from entry level to cutting edge products. The selection of the samples occurred randomly. na na 300 products from 16 product areas 100 cm2 lines placed on the market in four cutted in 2 mm x 2 industrial sectors (Coated metal mm, for the liquid wares, textile products, leather sample, 1 mL was products, household products) collected na Solids (coated materials): at least 200 cm2 or 2 g, solids (non- coated): sampled according to EN ISO 8130-9 see sampling Sample materials need to ground as appropriate to ensure an efficient extraction process. Textile and paper shall be cut into pieces of maximum 1 cm2 before methanol is added. For grinding of polymers and granulates it is recommended to use EN ISO 6427 or ISO 9113. 126 samples in four categories: Textiles, Floor coverings, Electrical & Electronic equipment and plastics. All bought in Czech Republic 5 g Materials were crushed, chopped or cut into small pieces Textile finishing agents (TFAs) samples were collected from both local and international brands na ultrasonic extraction A stock AFFF solution was obtained from a U.S. Air Force Base na 1:93,000 diluted AFFF solution 9 FT AFFF and 1 Class A foam (PFOS-CHEK, advertised as PFASfree) were purchased from commercial sources in 2018. na dilutions with Mili-Q water (10000x for non-targeted, 7500x for TF and IF, 50000x for EOF and targeted) 23 industry samples na UV-based TOP method as faster replacement of conventional heat-based TOP assay, diluted 1000-10,000 times auto_x0002_mated solid phase na na extraction (ASPE) Extraction Clean up solid and liquid sample extraction (Liu 2012, US EPA Report, EPA/600/R-12/585) na Samples were extracted with methanol for ionic compounds and ethyl acetate for neutral PFASs two times for 15 min in an ultrasonic bath with vortex treatment in between After centrifugation and solvent evaporation, an aliquot of1 mL extract was transferred for dispersive clean up with ENVICarb(50 mg, 1 mL, 100e400 mesh, Supelco, USA na na methanol for ionic compounds and ethylacetate for FTOH Centrifugation and solvent evaporation, clean up with ENVI-Carb and glacial acetic acid (for ionic PFAS) differ depending on the respective matrix: ion pair extraction, acidic- alkaine sequential extraction or SPE with acetone, hexane or methyl-tbutyl ether as solvent differ depending on the respective matrix ultrasonically with methanol filtration Sonification in methanol for textile, fabrics, leather and paper Concentrate the extract by a factor of 10 and use a clean-up if necessary. Active carbon clean-up and/or solid phase extraction (SPE) clean-up may be used. Transfer a known volume into a suitable LC sampling vial . If necessary dilute the original solution further and repeat the analysis Methanol with the addition of ammonium acetate Following extraction, samples were cleanedup according to the procedures for PFAAs analysis described indetail elsewhere (Karaskova et al., 2016). na na na na SPE; no extraction for TOP assay The extracts were blown to dryness using a nitrogen evaporator and reconstituted in 1 mL of LC-MS grade methanol and split between combustion ion chromatography (CIC) and LC-MS/MS. SPE according to EPA Method 537 na na na Measurement Quantification method HPLC/MS/MS internal standardisation using masslabeled standards UPLC-MS/MS and GC-MS internal standards UHPLC-Q-TOF-MS, in-house accurate-mass database and a mass spectral library na GC-MS internal standard PFAA: HPLC-MS/MS FTOH: GC/CI-MS internal standardisation using masslabeled internal standards The liquid chromatography-tandem mass spectrometry (LC-MS/MS) instrument used in this study was an Agilent 1290 infinity-6410A with a Zorbax Eclipse XDB C18 column (150 mm I.D, 2.1 mm length, 5.0 mm particle size). mass labeled internal standard, calibration curve LC-qMS, LC-tandemMS Quantify the samples by using the unextracted external calibration curve. When spiking with labelled reference solutions, the determination of the concentration is independent of possible errors made during injection. Also, errors caused by sample losses during distinct steps of sample pretreatment or the adjustment of final sample extract volume as well as matrix effects in the sample are accounted for. GC-MS internal standards gas chromatography mass spectrometry (GC-MS) TOP assay method UPLC-TOF-MS: targeted and Kendrick mass defect method mass-labeled internal standards A Sciex X500R Quadrupole Time-of-Flight MS (QToF/ MS) system using SWATH Data-Independent Internal standardisation using mass- Acquisition was operated in both positive and labeled standards and semi-quantification negative electrospray ionization (ESI+/-) mode for of 63 PFAS through suspect screening QToF-MS and MS/MS analysis. analysis TF/EOF/IF: CIC, TOP assay, LC-MS/MS (targeted), Non-targeted: UPLC with Thermo Orbitrap Fusion mass spectrometer Quantifiying oxidizable precursors using bayesian inference, Internal standardisation using mass-labeled standards for targeted analysis, TF and EOF: Concentrations were determined from the average peak areas of duplicate injections using an eight-point calibration curve of PFOA LC-MS/MS, (UPLC, Dionex UltiMate 3000, USA) combined with a tandem triple quadrupole mass spectrometry (MS/MS, AB isotope-labelled surrogate standards and SCIEX API 3200, Canada) internal standards LC-MSMS The TOP assay was employed to verify a material balance around the precursor compounds. This assay generates hydroxyl radicals by the thermal breakdown of persulfate under basic conditions (Houtz and Sedlak, 2012). isotopes Working range (ng/mL) As Matrices carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non- woven medical garments, floor waxes, food- contact paper, membranes for apparel, and na thread-sealant tapes na Textiles, carpets and food contact materials na plastic toys food contact paper, textile, fire fighting foam, water proofing agents and lubricants, paint, leather, carpets, non-stick ware, printed na circuit boards textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking na forms and ski waxes calibration 5, 10, 25, and 50.0 mg/L coated metal wares, textile products, leather products, and household products Method is applicable for a concentration range for Coated materials like paper, textile, leather, PFOS in the extract solution carpets, clothes and footwear, Non-coated of 0,5 g/l to 50 g/l. materials, liquids Textiles, matierials of wood and composite wood, plastics, foam, air conditioner na components. electronic components na textile na AFFF na AFFF na fluorocarbon surfactants (FSs) na water and foam Reported levels (ng/mL) Individual PFCAs: ND-2600 ng g-1 product PFOA: up to 0,914 g/m2 Other PFCAs: up to 1,022 g/m2 FTOHs: up to 373 g/m2 na PFOA: up to 2000 g/kg (ski waxes), up to 19 g/m2 (outdoor textiles), up to 15 g/m2 (baking paper) PFBA: up to 200 g/kg (leather) PFBS: up to 120 g/kg (leather) Of a total of 300 products, 51 were detected above the detection limits, which accounted for approximately 17% of the products tested. na Textiles: up to 77,6 g/kg Plastics: up to 0,384 g/kg OSB and wood: up to 18,3 g/kg (PFAS found in 14 out of 14 samples) Car interior materials: up to 3535 g/kg perfluorooctane sulfonate (0.37 mg/L) perfluorooctanoic acid (mean concentration: 0.29 mg/L), PFCAs by the TOP assay method was 58.83-3361.67 mg/L and 380.47-3156.07 mg/L, in ECF- and telomerization-based TFAs respectively Together, the target analytes and suspect structures are estimated to contribute 129 g/L of fluorine content to the diluted AFFF. EOF in PFAS-containing AFFF ranged from 220 to 840 mM F, Targeted PFAS explained 1% of EOF in FT AFFF PFCA concentrations before and after normal TOP assay were 0-4290 mg L-1 and 438-77,420 mg L-1, respectively. The PFCAs after 60 min UV-based TOP assay was 310-81,881 mg L-1 na info - validation of the method Limitations na na Recoveries of internal standards, procedural and instrumental blanks and methoddetection limits are regularly monitored as quality criteria for theanalysis na correlation coefficients all greater than 0.99 average mass devia_x0002_tions for the measurements over six consecutive days (one injec_x0002_tion per day) were lower than 3.41 ppm and 4.94 ppm for ABS and PVC plastic toy samples (RSDs) calcu_x0002_lated in terms of retention time and peak area were better than 1.0% for ABS toy sample and 6.2% for PVC inter-day precision tested in six consecutive days was better than 2.5% and 11.2% for ABS and PVC recovery: 61.2%-117.0% na As standard procedure, laboratory blanks, method detection limits (MDLs) and recoveries were examined. For each sample, a high resolution full scan spectra was used to control positive detections (typical mass tolerance 50 ppm). No laboratory contamination for any of the analyzed compound was detected na accreditations according to DIN EN ISO/IEC 17025:2005, quality control standards na linearity of the calibration curve, instrument detection limit (IDL), method detection limit (MDL), and quality control. na The recovery of labelled reference compound shall be in the range from 70 % to 125 % for the sample to be considered valid. The accuracy of method was evaluated using a set of spiked solidblank materials (polyurethane foam (n6) and sand matrix blank(n10)) na Calculated recoveries of the native standard were between 70% and 130%. The relative standard deviation of replicates was below 20% na na na Recoveries for each targeted PFAS 77 ranged from 72-130%, except for 8:2 FTSA (62%) and 10:2 FTSA (45%), TF: Relative standard deviations of duplicate injections <8% and method recovery 99%, EOF: relative standard deiations <5%, method recovery 96% The availability of analytical standards has not kept pace with the new PFAS in commerce, and the existence of chemical standards does not always immediately result in the expansion of common PFAS testing panels. na na recovery: 14-23% RSD 95% na LoD (ng/mL) subgroup Measurement - generic name na na The MDLs for individual substances ranged from 0.005 to0.010mgm2and 0.5 to 2mgm2for ionic and neutral PFASsrespectively. na LC-MS/MS LC-MS/MS, GC-MS 0.01-0.98 mg kg-1 na MDLs not reported na LC-HRMS GC-MS LOQ (PFAA) = 0.1-0.5 g/kg or 0.02-0.5 g/ m2 LOD (FTOH) = 20000 g/kg na LC-MS/MS, GC-MS MDLs between 0.47 and 1.42 mg/ L na LC -MS/MS na LC-MS/MS na na GC-MS 0,1-8,6 ng/mL na GC-MS, LC-HRMS not reported LC-HRMS Targeted: MDL = 2.78-38,86, 116.92 (PFTeDA), 131.88 (PFNS) nM F CIC, TOP assay, LC-HRMS na na LC-MS/MS na LC-MS/MS Title Authors Journal year Comments DOI link Multianalyte profiling of per- and polyfluoroalkyl substances (PFASs) in liquid commercial products Favreau et al. Chemosp here 2017 Also applied to AFFF 10.1016/ j.chemospher e.2016.11.127 Concentrations and trends of perfluorinated chemicals in potential indoor sources from 2007 through 2011 in the US Liu et al. Chemosp here 2014 na 10.1016/ j.chemospher e.2013.10.001 Are imported consumer products an important diffuse source of PFASs to the Norwegian environment? Vestergren et al. Environm ental Pollution 2015 na 10.1016/ j.envpol.2014. 12.034 ANALYSIS OF PFASs AND TOF Daniel Borg, IN PRODUCTS Jenny Ivarsson 2017 na na Survey of perfluoroalkyl acids (PFAAs) and their precursors present in Japanese consumer products Ye et al. Chemosphe 2015 targeted Suspect screening of 200 hazardous substances in plastic toys using ultra-high- performance liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry Meng et al. J Chromato 2020 na Perfluoroalkyl and polyfluoroalkyl substances (PFASs) in consumer productsin Norway - A pilot study Herzke et el. Chemosp here 2012 na 10.1016/ j.chemospher e.2015.02.026 10.1016/ j.chroma.2019 .460830 10.1016/ j.chemospher e.2012.03.035 Perfluoroalkyl and polyfluoroalkyl substances in consumer products Kotthoff et al. Survey of perfluorinated compounds in consumer products by liquid chromatography-tandem mass spectrometry Lee et al. Environ Sci Energy & Environm ent 2020 Vol. 31 Issue 4 Pages 713-729 2015 na 2019 na 10.1007/s1135 10.1177/0958 305x1988237 6 CEN/TS 15968:2010 Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LCqMS or LC-tandem/MS Also used for other matrices, sample 2010 treatmant different Screening for perfluoroalkyl acids in consumer products, building Chemosp materials and wastes Becanova et al. here 2016 na 10.1016/ j.chemospher e.2016.08.112 0045-6535/ How Do We Measure Poly- and Perfluoroalkyl Substances (PFASs) at the Surface of Environ Consumer Products?: Sci Environmental Science and Technol Technology LETTERS Tokranov et al. Lett 10.1021/ Method development acs.estlett.8b0 2019 for consumer products 0600 Screening of textile finishing agents available on the Chinese market: An important source of per- and polyfluoroalkyl substances to the environment Mumtaz et al. Frontiers of Environm ental Science & Engineeri ng 2019 Vol. 13 Issue 5 2019 na 10.1007/ s11783-0191145-0 Analysis and characterization of novel fluorinated compounds used in surface treatments products Frederiksson et al. Chemosp here 2022 na https://www.sc PFAS CAS (if available in publication 41 targeted PFAs including PFCAs (C4-C16), PFSAs (C4, C6, C8, C10), ipPFNS, PFPAs (C6, C8, C10), FOSA, N-Me FOSA, N-Et FOSA, FASAAs: FOSAA, N-MeFOSAA, N- EtFOSAA, N-MeFOSE, N-EtFOSE, FTSAs (4:2, 6:2, 8:2 FTS), FTOHs (4:2, 6:2, 7:2s, 8:2, 10:2), 8:2 FTI, 8:2 FTAC, 8:2 FTMAC na 9 PFCAs (C4 to C12), 5 PFASs (C4, C6, C7, C8, C10) na C4-C14 PFCAs, C4, C6 ,C8 ,C10 PFSAs, 4:2, 6:2, 8:2 and 10:2 FTOHs, N-ethyl perfluorooctanesulfonamidoethanol (EtFOSE), N- Methyl perfluorooctane sulfona-midoethanol (MeFOSE), N-Ethyl perfluorooctane sulfonamide(EtFOSA) and N-Methyl perfluorooctane sulfonamide (MeFOSA) na Perfluorinated carboxylic acids (PFCAs): PFBA, PFHxA, PFOA, PFNA, PFDA. Perfluorinated sulfonic acids (PFSAs): PFBS, PFHxS, PFOS. Fluorotelomer alcohols (FTOHs): 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH. Fluorotelomer acrylates (FTAs): 6:2 FTA, 8:2 FTA, 10:2 FTA. Perfluorooctane sulphonamides (FOSAs): MeFOSA, EtFOSA. Perfluorooctane sulfonamidoethanols (FOSEs): MeFOSE, EtFOSE. Total Organic Fluorine (TOF). na Perfluoroalkane sulfonic acids (PFSAs), Precursors of perfluorooctane sulfonic acid (Precursors of PFOS) Perfluorooctane sulfonamidoethanols (FOSEs), Perfluoroalkane sulfonamides (FASAs), Perfluoroalkane sulfonamidoacetic acids (FASAAs), Perfluoroalkyl carboxylic acids (PFCAs) - Precursors of perfluoroalkyl carboxylic acids (Precursors of PFCAs), Fluorotelomer unsaturated carboxylic acids (FTUCAs), Fluorotelomer carboxylic acids (FTCAs), Fluorotelomer sulfonic acid (FTSA) PPeerrfflluuoorroopaleknytlapnhooicspahcoidnic acid (PFPA) na Perfluorobutanesulfonic acid Perfluorohexanoic acid Perfluoroheptanoic acid Perfluorooctanoic acid Perfluorononanoic acid Perfluorooctanesulfonic acid Perfluorodecanoic acid Perfluoroundecanoic acid Perfluorododecanoic acid Pentacosafluorotridecanoic acid Perfluoromyristic acid Perfluoropalmitic acid Perfluorooctadecanoic acid na PFAS (i.e. C4-C14 PFCAs, C4,C6,C8,C10 PFSAs, 6:2 and 8:2 fluorotelomersulfonates (FTSs), PFOSA, 4:2, 6:2, 8:2, 10:2 FTOH na PFBA, PFPA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFTrA, PFTeA, PFBS, PFHxS, PFHpS, PFOS, PFDS, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, PFOSA na PFHXA, PFHpA, PFOA, PFNA, PFDA, PFBS, PFHxS, PFOS, PFOSA, N-MeFOSA, N-EtFOSO 307-24-4, 375-85-9, 335-67-1, 375-95-1, 335-76-2, 375-73-5, 355-46-4, 1763-23-1, 754-91-6, 31506-32-8, 4151-50-2 PFOS, PFOSA, N-Me-FOSA, N-Et-FOSA, N-Me-FOSE alcohol, N-Et-FOSE alcohol, PFOS salt 1763-23-1 (PFOS) 754-91-6 (PFOSA) 24448-09-7 (N-Me-FOSE alcohol) 1691-99-2 (N-Et-FOSE alcohol) PFPA, PFHxA, PFHpA, PFOA, PFNa, PFDA, PFUnDA, PFDoDa, PFTrDA, PFTeDA, PFBS, PFHxS, PFHpS, PFOS and PFDS na surficial fluorine content, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA, PFBS, PFHxS, PFOS, FOSA, 6:2 FtS, N-MeFOSAA, N-EtFOSAA na Targeted and non-targeted PFAS na FBSA, Me-FBSA, FHxSA, Me-FHxSA, FOSA, TFMS, PFEtS, PFPrS, PFBS, PFPeS, L-PFHxS, PFHpS, L-PFOS, PFNS, PFDS, PFDoDS, 4:2 FTSA, 6:2 FTSA, 8:2 FTSA, 3:3 FTCA, 5:3 FTCA, 7:3 FTCA, 6:2 FTUCA, 8:2 FTUCA, 10:2 FTUCA, TFA, PFPrA, PFBA, PFPeA, PFHxA, PFHpA, L-PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTDA, PFHxDA, PFOcDA, PFHxPA, PFOPA, PFDPA, 6:6 PFPiA, 6:8 PFPiA, 8:8 PFPiA, 11ClPF3OUdS, 9ClPF3ONS, T- PFECHS, C8-FASA-based copolymers, C4-FASA-based copolymers na Sampling sample amount used Pre- treatment Household products included impregnation agents (n = 60), cleansers (n = 24), polishes (n = 18), lubricants (n = 7). A miscellaneous category of products (n = 23) was defined by various applications that included foamsuppressing agents for the chromium industry, paints, ski wax, inks and tanning substances. 500 mg for LC-MS, 200 mg for GC-MS LC-MS: dissolved in 10 mL water, adding methanol/water, ammonium acetate (pH 4), GC- MS: dissolved in 10 mL methanol, filtration 95 samples from 35 consumer products including carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non- woven medical garments, floor waxes, food-contact paper, membranes for apparel, and thread-sealant tapes. They were purchased from retail outlets in the United States between March 2007 and September 2011. 5 x 5 cm solid products were cut into smaller subsections. Liquid products were subdivided into at least three 30-mL polypropylene vials 45 furniture textile, carpet, clothing and food contactmaterial samples were purchased from three major retail stores inTroms and Trondheim during the period November2012eFebruary 201 10 x 10 cm samples were cut into small pieces and spiked with masslabeled internal standard In total 17 products were randomly selected from shelves in a number of Swedish retail stores and supermarkets for analysis na na Five categories: car wash/coating products, sprays for fabrics and textiles, insecticides, rust inhibitors, and paints 50 mg na pulverized after freezing 0,2 g 30 products in 6 different product groups: waterproofing agents, paint, coated fabrics, non-stick ware, electronics and fire fighting agents. They were purchased from retailers in Norway and Sweden. 1 g dissolvation- precipitation of polymers Liquid and solid samples were homogenized 115 samples of consumer products including textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes. The individual samples analysed were bought from local retailers or collected by co-workers of the institute or local clubs (e.g. ski waxes from local skiing club). The sampled products span all quality levels from entry level to cutting edge products. The selection of the samples occurred randomly. na na 300 products from 16 product areas 100 cm2 lines placed on the market in four cutted in 2 mm x 2 industrial sectors (Coated metal mm, for the liquid wares, textile products, leather sample, 1 mL was products, household products) collected na Solids (coated materials): at least 200 cm2 or 2 g, solids (non- coated): sampled according to EN ISO 8130-9 see sampling Sample materials need to ground as appropriate to ensure an efficient extraction process. Textile and paper shall be cut into pieces of maximum 1 cm2 before methanol is added. For grinding of polymers and granulates it is recommended to use EN ISO 6427 or ISO 9113. 126 samples in four categories: Textiles, Floor coverings, Electrical & Electronic equipment and plastics. All bought in Czech Republic 5 g 94 consumer products that represent frequently used items on a college campus of Harvard University. These included: 45 food contact materials, 37 textiles, and 12 domestic products such as lens wipes, bandages, masks, and a shower curtain 1 0.03 g Materials were crushed, chopped or cut into small pieces cut using methanol-rinsed scissors, mounted on carbon tape for XPS Textile finishing agents (TFAs) samples were collected from both local and international brands na Two technical mixtures of ScotchgardTM Pre-2002 formulation and ScotchgardTM Post-2002 formulation were purchased from AccuStandard Inc. na ultrasonic extraction target analysis: na Extraction Clean up LC-MS: SPE with methanol/ ammonium acetate (50:50) LC-MS: adding ammonium hydroxide in methanol (0.5 %), neutralized with acetic acid solid and liquid sample extraction (Liu 2012, US EPA Report, EPA/600/R-12/585) na Samples were extracted with methanol for ionic compounds and ethyl acetate for neutral PFASs two times for 15 min in an ultrasonic bath with vortex treatment in between After centrifugation and solvent evaporation, an aliquot of1 mL extract was transferred for dispersive clean up with ENVICarb(50 mg, 1 mL, 100e400 mesh, Supelco, USA na na The PFAS extraction procedure and instrumental analysis for all samples was based on a previous report (Zushi et al., 2012) na na na methanol for ionic compounds and ethylacetate for FTOH Centrifugation and solvent evaporation, clean up with ENVI-Carb and glacial acetic acid (for ionic PFAS) differ depending on the respective matrix: ion pair extraction, acidicalkaine sequential extraction or SPE with acetone, hexane or methyl-tbutyl ether as solvent differ depending on the respective matrix ultrasonically with methanol filtration Sonification in methanol for textile, fabrics, leather and paper Concentrate the extract by a factor of 10 and use a clean-up if necessary. Active carbon clean-up and/or solid phase extraction (SPE) clean-up may be used. Transfer a known volume into a suitable LC sampling vial . If necessary dilute the original solution further and repeat the analysis Methanol with the addition of ammonium acetate Following extraction, samples were cleanedup according to the procedures for PFAAs analysis described indetail elsewhere (Karaskova et al., 2016). methanol extraction, XPS (not extracted sample/ methanol extract) na na na target analysis: na TOP assay: remaining side-chain fluorinated copolymer were extracted after oxidation with MTBE target analysis: na Measurement Quantification method internal standardisation using massLC- MS/MS, GC-MS/MS for FTOHs, FTI, FTAC, FTMAC labeled standards HPLC/MS/MS internal standardisation using masslabeled standards UPLC-MS/MS and GC-MS internal standards Lc-MSMS and combustion-IC na Fluor was determined by Ion chromatography after thermal decomposition internal standards UHPLC-Q-TOF-MS, in-house accurate-mass database and a mass spectral library na GC-MS internal standard PFAA: HPLC-MS/MS FTOH: GC/CI-MS internal standardisation using masslabeled internal standards The liquid chromatography-tandem mass spectrometry (LC-MS/MS) instrument used in this study was an Agilent 1290 infinity-6410A with a Zorbax Eclipse XDB C18 column (150 mm I.D, 2.1 mm length, 5.0 mm particle size). mass labeled internal standard, calibration curve LC-qMS, LC-tandemMS GC-MS Quantify the samples by using the unextracted external calibration curve. When spiking with labelled reference solutions, the determination of the concentration is independent of possible errors made during injection. Also, errors caused by sample losses during distinct steps of sample pretreatment or the adjustment of final sample extract volume as well as matrix effects in the sample are accounted for. internal standards X-ray photoelectron spectrosopy (XPS), LC-(-)ESI-MS, LC-QTOF-MS internal standards gas chromatography mass spectrometry (GC-MS) TOP assay method UPLC-TOF-MS: targeted and Kendrick mass defect method mass-labeled internal standards target analysis: UPLC-MS/MS target analysis: SFC-MS/MS (ultra-short chain acids C1-C3) TOP assay method QTOF MS analysis (side-chain fluorinated copolymer) total fluorine: TF analysis using CIC semi-quantification of new PFAS based on the average responses of the adjacent compounds or by analyzing a small number of compounds from the group at known concentrations Working range (ng/mL) As Matrices household products (impregnation agents, cleanser, polishes), lubricants, foamsuppressing agents for the chromium industry, paints, ski waxes, inks, tanning na substances, carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non- woven medical garments, floor waxes, food- contact paper, membranes for apparel, and na thread-sealant tapes na Textiles, carpets and food contact materials na na na surfactant containing consumer products na plastic toys food contact paper, textile, fire fighting foam, water proofing agents and lubricants, paint, leather, carpets, non-stick ware, printed na circuit boards textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking na forms and ski waxes calibration 5, 10, 25, and 50.0 mg/L coated metal wares, textile products, leather products, and household products Method is applicable for a concentration range for Coated materials like paper, textile, leather, PFOS in the extract solution carpets, clothes and footwear, Non-coated of 0,5 g/l to 50 g/l. materials, liquids Textiles, matierials of wood and composite wood, plastics, foam, air conditioner na components. electronic components N7A paper and textile na textile na sediment and technical mixtures Reported levels (ng/mL) 55% of all samples contained at least one PFAS between 0.1 and 25'000 mg/kg of product, with the majority of products falling within the 100e1000 mg/ kg range Individual PFCAs: ND-2600 ng g-1 product PFOA: up to 0,914 g/m2 Other PFCAs: up to 1,022 g/m2 FTOHs: up to 373 g/m2 several orders of magnitude for the products collected 2014, 2015 and 2016, respectively, from g/m2 to g/m2 g highest concentration of TOF were dental floss (310 g/kg), non-stick baking ware (1.7 g/ m2) and table cloth (0.9 g/m2). , g/l to mg/l, and g/kg to g/kg high total concentrations of PFAAs and their precursors were found in sprays for fabrics and textiles: 30 000 ng g-1 and car wash/coating products 7500 ng g-1 na PFOA: up to 2000 g/kg (ski waxes), up to 19 g/m2 (outdoor textiles), up to 15 g/m2 (baking paper) PFBA: up to 200 g/kg (leather) PFBS: up to 120 g/kg (leather) Of a total of 300 products, 51 were detected above the detection limits, which accounted for approximately 17% of the products tested. na Textiles: up to 77,6 g/kg Plastics: up to 0,384 g/kg OSB and wood: up to 18,3 g/kg (PFAS found in 14 out of 14 samples) Car interior materials: up to 3535 g/kg PFOA: 3200 nmol m-2 (0.38 mg kg-1) (carpet), PFBA: 960 nmol m-2 (0.60 mg kg-1) (disposable bowl), 45% F from a new upholstery sample perfluorooctane sulfonate (0.37 mg/L) perfluorooctanoic acid (mean concentration: 0.29 mg/L), PFCAs by the TOP assay method was 58.83-3361.67 mg/L and 380.47-3156.07 mg/L, in ECF- and telomerization-based TFAs respectively The technical mixtures stated concentration of 100 g mL- 1 showed a fluorine content of 0.41-0.60% for Pre-2002 and 1.7-1.9% for Post-2002 info - validation of the method na Limitations na na na Recoveries of internal standards, procedural and instrumental blanks and methoddetection limits are regularly monitored as quality criteria for theanalysis na na na Compounds with a recovery outside of the range of 50-150% were removed from this report. Procedural blank sam_x0002_ples (n = 3) were prepared and analyzed na correlation coefficients all greater than 0.99 average mass devia_x0002_tions for the measurements over six consecutive days (one injec_x0002_tion per day) were lower than 3.41 ppm and 4.94 ppm for ABS and PVC plastic toy samples (RSDs) calcu_x0002_lated in terms of retention time and peak area were better than 1.0% for ABS toy sample and 6.2% for PVC inter-day precision tested in six consecutive days was better than 2.5% and 11.2% for ABS and PVC recovery: 61.2%-117.0% na As standard procedure, laboratory blanks, method detection limits (MDLs) and recoveries were examined. For each sample, a high resolution full scan spectra was used to control positive detections (typical mass tolerance 50 ppm). No laboratory contamination for any of the analyzed compound was detected na accreditations according to DIN EN ISO/IEC 17025:2005, quality control standards na linearity of the calibration curve, instrument detection limit (IDL), method detection limit (MDL), and quality control. na The recovery of labelled reference compound shall be in the range from 70 % to 125 % for the sample to be considered valid. The accuracy of method was evaluated using a set of spiked solidblank materials (polyurethane foam (n6) and sand matrix blank(n10)) na Duplicate injection, precision experiments na Calculated recoveries of the native standard were between 70% and 130%. The relative standard deviation of replicates was below 20% na na na LoD (ng/mL) subgroup Measurement - generic name LOQ: 0.5-2 ng/mL (LC-MS), 2-10 ng/ mL (GC-MS) na LC- MS/MS, GC-MS/MS na na The MDLs for individual substances ranged from 0.005 to0.010mgm2and 0.5 to 2mgm2for ionic and neutral PFASsrespectively. na LC-MS/MS LC-MS/MS, GC-MS na na LC-MS/MS, IC 2 ng g_x0003_1 na IC 0.01-0.98 mg kg-1 na MDLs not reported na LC-HRMS GC-MS LOQ (PFAA) = 0.1-0.5 g/kg or 0.02-0.5 g/ m2 LOD (FTOH) = 20000 g/kg na LC-MS/MS, GC-MS MDLs between 0.47 and 1.42 mg/ L na LC -MS/MS na LC-MS/MS na na GC-MS 1% for XPS, 0.063-3.7 ng g-1 (MQL) for LC-MS/ MS XPS, LC-MS/MS, LC-HRMS 0,1-8,6 ng/mL na GC-MS, LC-HRMS na na LC-MS/MS, SFC-MS/MS, LC-HRMS, CIC Title CEN/TS 15968:2010 - Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LCqMS or LC-tandem/MS Perfluoroalkyl and polyfluoroalkyl substances in consumer products Analysis of per- and polyfluorinated substances in articles Analysis of PFASs and TOF in products Levels of per- and polyfluoroalkyl substances (PFAS) in ski wax products on the market in 20 PFAS i kemiska produkter och varor Ett tillsynsprojekt med fokus p POPs-frordningens begrnsningar av PFOA och PFOS (PFAS in chemical products and articles A regulatory project focusing on the POPs Regulation restrictions on PFOA and PFOS) Perfluoroalkyl and polyfluoroalkyl substances (PFASs) in consumer productsin Norway - A pilot study Authors Journal year Standard Kotthoff et al. na Environ Sci Pollut Res Int 2010 2015 Blom et al. Borg et al. Nordic Council of Ministers 2015 Nordic Council of Ministers 2017 Fang et al. KEMI Herzke et el. Environmental Science: Processes & Impacts 2019 na 2021 Chemosphere 2012 comments DOI link Also used for other matrices, sample treatmant different na na 10.1007/s11356-015-4202-7 na http://dx.doi.org/10.6027/na2015-911 na http://dx.doi.org/10.6027/ na Several matrices tested: Textiles, Ski wax, and other consumer products 10.1039/d0em00357c na na 10.1016/j.chemosphere.2012.03.035 name PFOS, PFOSA, N-Me-FOSA, N-Et-FOSA, N-Me-FOSE alcohol, N-Et-FOSE alcohol, PFOS salt PFBA, PFPA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUna, PFDoA, PFTrA, PFTeA, PFBS, PFHxS, PFHpS, PFOS, PFDS, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, PFOSA PFCAs (PFBA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA), PFASs (PFBS, PFHxS, PFOS), PAPs (6:2 diPAP, 6:2 monoPAP, 8:2 diPAP, 8:2 mono-PAP), FTOH (4:2, 6:2, 8:2), FTS (4:2, 6:2) TOF, targeted analysis of PFCAs (PFBA, PFHxA, PFOA, PFna, PFDA), PFSAs (PFBS, PFHxS, PFOS), FTOHs (4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH), FTAs (6:2 FTA, 8:2 FTA, 10:2 FTA), FOSAs (MeFOSA, EtFOSA), FOSEs (MeFOSE, EtFOSE) Perfluorobutanoic acid (PFBA, C4) Perfluoropetanoic acid (PFPeA, C5) Perfluorohexanoic acid (PFHxA, C6) Perfluoroheptanoic acid (PFHpA, C7) Perfluorooctanoic acid (PFOA, C8) Perfluorononanoic acid (PFna, C9) Perfluorodecanoic acid (PFDA, C10) Perfluoroundecanoic acid (PFUnDA, C11) Perfluorododecanoic acid (PFDoDA, C12) Perfluorotridecanoic acid (PFTrDA, C13) Perfluorotetradecanoic acid (PFTeDA, C14) Perfluoropentadecanoic acid (PFPeDA, C15) Perfluorohexadecanoic acid (PFHxDA, C16) Perfluoroheptadecanoic acid (PFHpDA, C17) Perfluorooctadecanoic acid (PFODA, C18) Perfluorononadecanoic acid (C19) Perfluoroeicosanoic acid (C20) Perfluoroheneicosanoic acid (C21) Perfluorodocosanoic acid (C22) Perfluorotetracosanoic acid (C23) Perfluorotricosanoic acid (C24) Perfluoropentacosanoic acid (C25) PFAS Tests according to CEN/TS 15968:2010 EOF not further described PFAS (i.e. C4-C14 PFCAs, C4,C6,C8,C10 PFSAs, 6:2 and 8:2 fluorotelomersulfonates (FTSs), PFOSA, 4:2, 6:2, 8:2, 10:2 FTOH CAS (if available in source) 1763-23-1 (PFOS) 754-91-6 (PFOSA) 24448-09-7 (N-Me-FOSE alcohol) 1691-99-2 (N-Et-FOSE alcohol) na 375-22-4 (PFBA), 307-24-4 (PFHxA), 375-85-9 (PFHpA), 335-67-1 (PFOA), 375-95-1 (PFna), 33576-2 (PFDA), 4234-23-5 (PFUnDA), 307-55-1 (PFDoDA), 72629-94-8 (PFTrDA), 376-06-7 (PFTeDA), 29420-49-3 (PFBS salt), 3871-99-6 (PFHxS salt), 1763-23-1 (PFOS salt), 2043-47-2 (4:2 FTOH), 647-42-7 (6:2 FTOH), 678-39-7 (8:2 FTOH), 57677-95-9 (6:2 diPAP), 57678-01-0 (6:2 monoPAP), 678-41-1 (8:2 diPAP), 57678-03-2 (8:2 mono-PAP), 757124-72-4 (4:2 FTS), 2942049-3 (6:2 FTS) 375-22-4 (PFBA), 2942049-3 (PFBS salt), 307-24-4 (PFHxA), 3871-99-6 (PFHxS salt), 2043-47-2 (4:2 FTOH), 757124-72-4 (4:2 FTS), 335-67-1 (PFOA), 1763-23-1 (PFOS salt), 647-42-7 (6:2 FTOH), 29420-49-3 (6:2 FTS), 31506-32-8 (MeFOSA), 4151-50-2 (EtFOSA), 2448-09-7 (MeFOSE), 1691-99-2 (EtFOSE), 37595-1 (PFna), 335-76-2 (PFDA), 678-39-7 (8:2 FTOH) na Tests according to CEN/TS 15968:2010 na Sampling sample amount used Liquids: method which will provide a representative sample of the liquid to be tested. see sampling 115 samples of consumer products including textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes. The individual samples analysed were bought from local retailers or collected by co-workers of the institute or local clubs (e.g. ski waxes from local skiing club). The sampled products span all quality levels from entry level to cutting edge products. The selection of the samples occurred randomly. na In total 29 different samples were analysed. The sampling was concentrated on a few but wide variety of household products, such as cleaning products and polishes for indoor use and for cars and sprays to waterproof shoes or clothes, food contact paper and baking forms included some products less commonly analysed, such as ski wax, dental floss and tablecloths. The samples were purchased in the vicinity of Oslo in supermarket chains that are found all over Norway. depending on the article: 0.05 mL, 71.5-100 cm^2 or 0.02-0.16 g In total 17 products were randomly selected from shelves in a number of Swedish retail stores and supermarkets for analysis (Cupcake forms, microwave popcorn bag, rinse aid, waterproofing shoe treatment, waterproofing textile treatment, shoe wax, floor polish, furniture polish, car wax). In total 29 samples of consumer products were collected in the previous study (including food contact material, textiles, lubricants, car wax, table cloth, ski wax and more) Pressed pellets of 100-120 mg for TOF 11 separate commercially available and best-selling ski wax products were purchased from one of Norway's largest sports stores in the summer of 2019. The ski wax products comprised; 3 wax blocks, 1 liquid wax and 7 powders. 10 mg Tests according to CEN/TS 15968:2010 Tests according to CEN/TS 15968:2010 30 products in 6 different product groups: waterproofing agents, paint, coated fabrics, non-stick ware, electronics and fire fighting agents. They were purchased from retailers in Norway and Sweden. 1 g Pre- treatment Dilution for AFFF: Pre-dilute the sample in separate steps with purified water or methanol (1:10 v/v, 1:100 v/v, 1:1 000 v/v) and mix sufficiently (e.g. 500 l sample into 4 500 l diluent). Ensure that there is no phase-separation in the sample. If necessary centrifuge the sample to precipitate non soluble particles. Dilute the pre-diluted sample 1:10 with water or methanol and an appropriate volume of internal standard solution (e.g. 100 l diluted sample, 100 l reference solution, 800 l water or methanol) to have in every dilution (1:10 v/v, 1:100 v/v, 1:1 000 v/v) the same concentration of the internal standard. Transfer an aliquot to a LC vial and analyse the sample. If high PFOS concentrations are expected, begin with the highest dilution (1:10 000 v/v) to avoid a carry over. na vortexing in methanol sample was homogenized, shredded for TOF na Tests according to CEN/TS 15968:2010 Liquid and solid samples were homogenized Extraction Clean up no extraction na differ depending on the respective matrix: ion pair extraction, differ depending acidic-alkaine sequential extraction or SPE with acetone, hexane on the respective or methyl-t-butyl ether as solvent matrix ultrasonification in methanol volume reduced to 2 mL, aliquot filtered LC-MS: ultrasonic extraction with matrix dependent solvents (no LC-MS: (multi)- further information), burning for TOF and absorbtion of step-sample clean- combustion gases in buffer solution up 10 mg (accurately weighed) of ski wax spiked with 0.5 ng of internal standards was extracted with 5 mL methanol. The wax/ methanol mixture was vortexed and extracted in an ultrasonic bath for 20 min and then stored at room temperature overnight. The mixture was placed in an ultrasonic bath for 20 min again the next day and then centrifuged (3000 rpm, 10 min) to facilitate sedimentation of the extracted solids. A 4 mL aliquot of the supernatant was transferred to a 13 mL polypropylene tube. The extraction of ski wax was repeated and the supernatant solutions combined. Following extraction, the 8 mL of supernatant was evaporated to approximately 200 L and 25 L recovery standard (M8PFOS and M8PFOA, both 20 pg L-1) and 200 L 4 mM NH4OAc in water were added. The extracts were then transferred to a polypropylene (PP) centrifuge tube with a nylon membrane filter and centrifuged at 13000 rpm for 5 min. The filtered extract was transferred to an autosampler vial and stored at 4 C until analysis. na Tests according to CEN/TS 15968:2010 Tests according to CEN/TS 15968:2010 methanol for ionic compounds and ethylacetate for FTOH Centrifugation and solvent evaporation, clean up with ENVI-Carb and glacial acetic acid (for ionic PFAS) Measurement LC-qMS, LC-tandemMS PFAA: HPLC-MS/MS FTOH: GC/CI-MS UPLC-MS/MS for ionic PFAS and PAP, GC/MSD for FTOH Targeted analysis with LC/MS-MS (Agilent HPLC 1290 Infinity Serie coupled with Agilent 6460A Triple Quad LC/MS-MSMS), TOF by IC PFAS were quantified using an ultra-performance liquid chromatography-tandem mass spectrometer (UPLC-MS/MS) instrument (Waters, ACQUITY-UPLC/XEVO-TQS) fitted with a BEH C18 column (1.7 m particles, 2.1 50 mm; waters). The mass spectrometer (MS) was operated in negative electrospray ionization multiple reaction monitoring (MRM) mode with the following MS parameters: capillary voltage 1100 V; nebulizer gas flow at 7 bars; desolvation gas flow at 600 L h-1; cone gas flow at 150 L h-1. The desolvation temperature was 350 C. The m/z cone voltages and collision energies used for each PFAS are listed in Table S2. Tests according to CEN/TS 15968:2010 GC-MS Quantification method Quantify the samples by using the unextracted external calibration curve. When spiking with labelled reference solutions, the determination of the concentration is independent of possible errors made during injection. Also, errors caused by sample losses during distinct steps of sample pre-treatment or the adjustment of final sample extract volume as well as matrix effects in the sample are accounted for. internal standardisation using mass-labeled internal standards internal standardisation using mass-labeled internal standards LC-MS: internal isotope-labeled standards (isotope dilution method) Quantification of all target analytes was performed using an internal standard calibration curve with nine points (0.008-150 ng mL-1, R2 > 0.99). Stable isotope mass labelled internal standards were available for C4-C6 and C8-C12 PFCAs, as well as for PFHxS and PFOS. C7 and C13-25 PFCAs, PFBS and PFDS were quantified using 13C2-perfluorohexanoic acid (PFHxA), 13C2-perfluorododecanoic acid (PFDoDA), 18O2-perfluorohexane sulfonate acid (18O2-PFHxS) and 13C4perfluorooctane sulfonate acid (13C4-PFOS) as internal standards, respectively. Reference standards for native C15, C17 and C19-25 PFCAs were not available. Therefore, for quantification of C15, C17 and C19-25 PFCAs the relative response factors (relative to 13C2-PFDoDA) were calculated from the calibration curves of C14, C16 and C18 PFCAs, respectively. All reported concentrations for C15, C17 and C19-25 PFCAs should thus be considered as semi-quantitative estimates due to the lack of authentic native standards for these compounds. The method detection limit (MDL) was defined as the lowest calibration point concentration resulting in a signal-to-noise ratio of three, if the specific PFAS were not detected in the blanks. For the analytes which were detected in the blanks, MDLs were defined as the mean blank concentration plus three times the standard deviation of the blank. Tests according to CEN/TS 15968:2010 internal standard LoD (ng/mL) subgroup Measurement - generic name na na LOQ (PFAA) = 0.1-0.5 g/ kg or 0.02-0.5 g/m2 LOD (FTOH) = 20000 g/ kg na LC-MS/MS LC-MS/MS, GC-MS LOD = 0.03-0.15 g/m2, only qualitative for 6:2 monoPAP, 8:2 PAP, 6:2 diPAP, 8:2 diPAP na TOF: About 10 pellets must be processed to sustain a LOQ of 1 mg/kg fluorine (LOQ fluoride = 0.1 mg/l for IC) na LC-MS/MS, GC-MS LC-MS/MS , CIC 0.1-2.5 ng g-1 na LC-MS/MS Tests according to CEN/TS 15968:2010 Tests according to CEN/TS 15968:2010 MDLs not reported na GC-MS Title Authors Journal Surface-enhanced Raman scattering (SERS) detection of fluorosurfactants in firefighting foams Fang et al. RSC Advances Potentiometric detection of AFFFs based on MIP Fang et al. Environmental Technology & Innovation Removal of Per- and Polyfluoroalkyl Substances (PFASs) in Aqueous Film-Forming Foam (AFFF) Using Ion-Exchange and Nonionic Resins Fang et al. Environ Sci Technol Reconstructing the Composition of Per- and Polyfluoroalkyl Substances in Contemporary Aqueous Film-Forming Foams Ruyle et al. Environ Sci Technol Lett Determination of total oxidizable precursors in foam surfactants and foam contaminated water based on UV-activated persulfate oxidation Fan et al. Sci Total Environ Assessment of PFAS fate, transport, and treatment inhibition associated with a simulated AFFF release within a WASTEWATER treatment plant Gonzalez et al. Chemosphere 262: 127900. Spatial Trends of Anionic, Zwitterionic, and Cationic PFASs at an Environ. Sci. Technol. AFFF-Impacted Site Nickerson et al. 2021, 55, 1, 313-323 Chemical Characterization of a Legacy Aqueous Film-Forming Foam Sample and Developmental Toxicity in Zebrafish (Danio rerio) Annunziato et al. Environ Health Perspect Characterization of the Chemical Contents of Fluorinated and Fluorine-Free Firefighting Foams Using a Novel Workflow Combining Nontarget Screening and Total Fluorine Analysis Dubocq et al. Environ Sci Technol Rapid Characterization of Emerging Per- and Polyfluoroalkyl Substances in Aqueous Film-Forming Foams Using Ion Mobility Spectrometry-Mass Spectrometry Rejection of per- and polyfluoroalkyl substances (PFASs) in aqueous film-forming foam by high-pressure membranes Luo et al. Liu et al. Environ Sci Technol Water Res A profile analysis with suspect screening of per- and polyfluoroalkyl substances (PFASs) in firefighting foam impacted waters in Okinawa, Japan Yukioka et al. Water Research Per- and Polyfluoroalkyl Substances in Representative Fluorocarbon Surfactants Used in Chinese Film-Forming Foams: Levels, Profile Shift, and Environmental Implications Mumtaz et al. Gas-Phase Detection of Fluorotelomer Alcohols and Other Oxygenated Per- and Polyfluoroalkyl Substances by Chemical Ionization Mass Spectrometry Riedel et al. Environmental Science & Technology Letters Environ Sci Technol Lett A new method to search for per- and polyfluoroalkyl substances (PFASs) by linking fragmentation flags with their molecular ions by drift time using ion mobility spectrometry Yukioka et al. Chemosphere Deep seepage of per- and polyfluoroalkyl substances through the soil of a firefighter training site and subsequent groundwater contamination Dauchy et al. Chemosphere Discovery of 40 Classes of Per- and Polyfluoroalkyl Substances in Historical Aqueous Film-Forming Foams (AFFFs) and AFFF- Barzen-Hanson et Impacted Groundwater al. Environ Sci Technol Per- and polyfluoroalkyl substances in firefighting foam concentrates and water samples collected near sites impacted by the use of these foams Dauchy et al. Chemosphere Multianalyte profiling of per- and polyfluoroalkyl substances (PFASs) in liquid commercial products Favreau et al. Chemosphere Chemical oxidization of some AFFFs leads to the formation of 6:2FTS and 8:2FTS Fang et al. Environmental Toxicology and Chemistry Identification of Novel Fluorinated Surfactants in Aqueous Film Environmental Science & Forming Foams and Commercial Surfactant Concentrates D'Agostino et al. Technology Zwitterionic, Cationic, and Anionic Fluorinated Chemicals in Aqueous Film Forming Foam Formulations and Groundwater from U.S. Military Bases by Nonaqueous Large-Volume Injection HPLC-MS/MS Backe et al. Environmental Science & Technology Persistence of perfluoroalkyl acid precursors in AFFF-impacted groundwater and soil Houtz et al. Environmental science & technology Organic fluorine content in aqueous film forming foams (AFFFs) and biodegradation of the foam component 6 : 2 fluorotelomermercaptoalkylamido sulfonate (6 : 2 FTSAS) Weiner et al. Environmental Chemistry Identification of Novel Fluorochemicals in Aqueous FilmForming Foams Used by the US Military Place et al. Environmental Science & Technology CEN/TS 15968:2010 - Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LCqMS or LC-tandem/MS na Total oxidisable precursor assay towards selective detection of PFAS in AFFF Amin et al. Journal of Cleaner production Perfluoroalkyl and polyfluoroalkyl substances (PFASs) in consumer productsin Norway - A pilot study Herzke et el. Chemosphere year Comments DOI link 2016b method development for pre- screening 10.1039/C5RA26114G 2016a method development for pre- screening 10.1016/j.eti.2015.12.003 2021 Focus on removal of PFAS 10.1021/acs.est.1c00769 2021 EPA method 10.1021/acs.estlett.0c00798 2021 na 2021 na 10.1016/ j.scitotenv.2020.142943 10.1016/ j.chemosphere.2020.127900 2021 na 10.1021/acs.est.0c04473 Modified EPA Method 537.1 for targeted PFAS by Eurofins, in publication only non2020 targeted method is discussed 10.1289/EHP6470 2020 na 2020 na 2020 na 10.1021/acs.est.9b05440 10.1021/acs.est.0c04798 10.1016/ j.watres.2020.116546 2020 na 10.1016/ j.watres.2020.116207 2019 according to EPA Method 537 10.1021/acs.estlett.9b00154 2019 10.1021/acs.estlett.9b00196 New method of linking fragment ions with their molecular ions by drift time using ion mobility spectrometry for PFAS based 2019 on fragmentation flagging 10.1016/ j.chemosphere.2019.124644 2019 na 10.1016/ j.chemosphere.2018.10.003 Also applied to consumer products and groundwater 2017 (other sample treatment) 10.1021/acs.est.6b05843 Also applied to water samples 10.1016/ 2017 from AFFF impacted sites j.chemosphere.2017.05.056 Also applied to consumer 2017 products, lubricants 10.1016/ j.chemosphere.2016.11.127 2015 na 2014 na 10.1002/etc.3115 10.1021/es403729e 2013 na 10.1021/es3034999 2013 na 10.1021/es4018877 2013 na 2012 na 10.1071/en13128 10.1021/es301465n Also used for other matrices, 2010 sample treatmant different na Recommendations for enhancement of the TOP 2021 assay are also provided 10.1016/ j.jclepro.2021.129568 2012 na 10.1016/ j.chemosphere.2012.03.035 PFAS PFOA, PFOS, 6:2 FTS CAS (if available in publicat na PFOA, PFOS, 6:2 FTS na 48 targeted PFAS (12 found: PFCAs (n = 3-7), PFSAs (n = 3-8), Cl-PFSA (n = 8)) and 63 semi- quantificated PFAS including AmPr-FASA (n = 2-6), AmPr-FASA-PrA (n = 2-6), CEtAmPr-FASA-PrA (n = 2-6), Cl-PFSA (n = 4-6), CMeAmPr-FASA (n =4-6), CMeAmPr-FAS-PrA (n = 3-6), F5S-PFAS (n = 6), FASA (n = 4,6), PFCAs (n = 5), PFSAs (n = 3,4,6,7,8,10), UPFAS (n = 7,8), KPFAS (n = 5-8), MeEtCMeAmPr-FAAd (n = 4), MeFASAA (n = 5, 6), OAmPr-FASA (n = 5,6), O-PFAS (n = 5,6), PFASi (n = 4-6), PFCPeCA (n = 6), TAmPr-FASA (n = 3-6), TAmPr-FASAPrA (n = 3-6), UPFSA (n = 6-8) and 63 semi-quantificated PFAS na 27 targeted PFAS including PFCAs (PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA), PFSAs (PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS), FTSAs (4:2, 6:2, 8:2, 10:2), FBSA, FHxSA, FOSA, non-targeted PFAS, TF (total fluorine), EOF (extractable orgonofluorine), IF (inorganic fluorine), TOP (total oxidizable precuror) identified PFAS: 1513864-10-2 (6:2 FTSAS-sulfoxide), 88992-45-4 (6:2 FTSHA), 88992-47-6 (6:2 FTSAS), 6497210-7 (6:2 FTTh-PrAm), 27619-97-2 (6:2 FTSA), 34455-29-3 (6:2 FTSA-PrB), 8047532-7 (6:2 FTNO), 76201-56-4 (EtOHAm-Pr-PFHxSAPrS), 1513864-18-9 (6:2 FTSO-OHPrTAm) Targeted PFCAs before/after TOP asssay na na na anionic, zwitterionic, and cationic poly- and perfluoroalkyl substances (PFASs) na 100 non-targeted PFAS, 26 targeted PFAS: PFOS, PFHxS, PFPeS, PFBS, PFHpS, PFHxA, PFOA, PFPeA, PFHpA, PFBA, PFNS, PFDS, FOSA, PFNA, PFDA, PFUnA, PFDoA, PFTriA, PFTeA, NMeFOSAA, NEtFOSAA, 4:2 FTS, 6:2 FTS, 8:2 FTS, Perfluoro-1- hexanesulfonamide, N-(3-(Dimethylamino) propyl)tridecafluoro hexanesulphonamide na Non-targeted, 17 targeted PFASs: PFBA, PFPeA, PFBS, PFHxA, PFHpA, PFHxS, PFOA, 6:2 FTSA, PFNA, PFOSA, PFOS, PFDA, PFUnDA, PFDS, PFDoDA, PFTrDA, PFTDA, PFHxDA, PFOcDA, total fluorine/ inorganic fluorine na Non-targeted na Targeted analysis of 10 PFASs, suspect screening na na na Taregted: PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, 4:2 FTS, 6:2 FTS, 8:2 FTS na 4:2, 6:2, 8:2, and 10:2 FTOH, PFOA, PFBA, HFPO- DA na Targeted analysis of 34 PFASs (12 PFCAs, 3 PFSAs, 3 PAPs, 3 FTSs, 5 FTCAs, 3 FTUCAs, 3 FASAs, 2 FASAAs) na 11 PFCAs (CnF2n1COO_x0003_, n 3e13), 5 PFSAs (CnF2n1SO3 _x0003_, n 4, 6, 7, 8, 10), 3 n:2 FTSAs (CnF2n1C2H4SO3 _x0003_, n 4, 6, 8), 3 fluorotelomer carboxylic acids (n:2 FTCAs, CnF2n1 CH2COO_x0003_, n 6, 8, 10), 3 fluorotelomer unsaturated carboxylic acids (n:2 FTUCAs, CnF2nCHCOO_x0003_, n 6, 8, 10), 5:3 ACID (C5F11(CH2)2COO_x0003_), perfluorooctane sulfonamide (FOSA, C8F17SO2NH2), Perfluorooctane sulfonamidoacetic acid (FOSAA, C8F17SO2NHCH2COOH), N-Methyl perfluorooctane sulfonamido_x0002_acetic acid (MeFOSAA, C8F17SO2N(CH3)CH2COOH), N-Ethyl per_x0002_fluorooctane sulfonamidoacetic acid (EtFOSAA, C8F17SO2N(C2H5) CH2COOH), 6:2 Fluorotelomer sulfonamide alkylbetaine (6:2 FTAB, C6F13C2H4S(O)2N(H)C3H6N(CH3)2CH2CO2H) and 6:2 Fluorotelomer sulfonamide propyl N$N dimethylamine (6:2 FtSaAM, C6F13C2H4S(O)2N(H)C3H6N(CH3)2) na Non-targeted: 57 classes of PFASs (40 new classes with over 240 individual PFAS) including N-SP- FASA, N-SPAmP-FASA, N-SHOPAmP-FASA, N- SPHOEAmP-FASA, N-SPAmP-FASAPS, N- DiHOPAmHOB-FASA, N-diHOPAmHOB-FASAPS, N- HOEAmP-FASAPS, N-HOEAmP-FASE, N- HOEAmHOP-FASA, N-HOEAmP-FASA, N-TAmP-N- MeFASA, N-TAmP-FASA, N-TAmP-FASAP, N- CMAmP-FASAP, N-CMAmP-FASA, CHAmEt-FA, CMAmB-FA na 154 PFAS, 32 targeted PFAS including PFCAs (n = 3- 13), PFSAs (n = 4,6,7,8,10), FTSAs (4:2, 6:2, 8:2), FTCAs (6:2, 8:2, 10:2), FTUCAs (6:2, 8:2, 10:2), 5:3 ACID, FOSA, FOSAA, MeFOSAA, EtFOSAA, 6:2 FTAB, 6:2 FtSaAM, total concentration of PFAA precursors na 41 targeted PFAs including PFCAs (C4-C16), PFSAs (C4, C6, C8, C10), ipPFNS, PFPAs (C6, C8, C10), FOSA, N-Me FOSA, N-Et FOSA, FASAAs: FOSAA, N- MeFOSAA, N-EtFOSAA, N-MeFOSE, N-EtFOSE, FTSAs (4:2, 6:2, 8:2 FTS), FTOHs (4:2, 6:2, 7:2s, 8:2, 10:2), 8:2 FTI, 8:2 FTAC, 8:2 FTMAC na PFOS, PFOA, 6:2 FTS, 8:2 FTS na Non-targeted: 103 PFAS compounds in 22 classes with chain length from C3-C15 including PFAAB, FTSAB, FTSAS (6:2, 8:2), FTAB (4:2, 6:2, 8:2, 10:2, 12:2), FTB, FTSHA, PFASAC, PFASNO na 4:2 FtTAoS, 6:2 FtAoS, 8:2 FtTAoS, 6:2 FtTHN+. 6:2 FtSaB, 8:2 FtSaB, 10:2 FtSaB, 6:2 FtSaAm, 8:2 FtSaAm, 5:1:2 FtB, 7:1:2 FtB, 9:1:2 FtB, 5:3 FtB, 7:3 FtB, 9:3 FtB, 4:2 FtS, 6:2 FtS, 8:2 FtS, PFBSaAm, PFPeSaAm, PFHxSaAm, PFHpSaAm, PFOSaAm, PFBSaAmA, PFPeSaAmA, PFHxSaAmA, PFHpSaAmA, PFOSaAmA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrA, PFTeA na 22 PFAA precursors, transformation products, perfluorinated sulfonates and carboxylates including 6:2 FtS, 8:2 FtS, FOSA, PFNA, PFOA, PFHpA, PFHxA, PFPeA, PFBA, PFOS, PFHpS, PFHxS, PFBS na Total organofluorine, PFCAs (C4-14), PFSAs (C4, 6, 8-10), FTSA, FTSAS (4:2, 6:2, 8:2), 6 : 2 FTSAS- sulfoxide (FTSAS-SO) and sulfone (FTSASSO2), perfluorooctanesulfonamidoacetate (FOSAA), N- methyl perfluorooctanesulfonamidoacetate (MeFOSAA), N-ethyl perfluorooctanesulfonamidoacetate (EtFOSAA) and 6 : 2 fluorotelomer unsaturated acids (FTUCAs, 4 : 2, 6 : 2, 8:2, 10:2, 3:5, 5:3, 7:3) na temerization-based fluorinated surfactants including 4:2, 6:2, 8:2, and 10:2 fluorotelomer sulfonamide with dimethyl quaternary amine and carboxylic acid functional groups na PFOS, PFOSA, N-Me-FOSA, N-Et-FOSA, N-Me-FOSE alcohol, N-Et-FOSE alcohol, PFOS salt 1763-23-1 (PFOS) 754-91-6 (PFOSA) 24448-09-7 (N-MeFOSE alcohol) 1691-99-2 (N-Et-FOSE alcohol) Targeted PFCAs, PFSAs and fluorotelomer sulfonic acids before/after TOP asssay na PFAS (i.e. C4-C14 PFCAs, C4,C6,C8,C10 PFSAs, 6:2 and 8:2 fluorotelomersulfonates (FTSs), PFOSA, 4:2, 6:2, 8:2, 10:2 FTOH na Sampling sample amount used groundwater from Williamstown (Australia) spiked with PFOA na na na A stock AFFF solution was obtained from a U.S. Air Force Base na 9 FT AFFF and 1 Class A foam (PFOS-CHEK, advertised as PFAS-free) were purchased from commercial sources in 2018. na 23 industry samples na na na Soil and groundwater from an aqueous film- forming foam (AFFF)-impacted site na A legacy AFFF, a 3% application formula, was acquired through the MA-DEP. The formulation and manufacturer of this mixture were unknown. na A selection of firefighting foams from four categories was included in this study: (i) aqueous filmforming foams (AFFFs; n = 10), (ii) alcohol resistant aqueous film-forming foam (AR- AFFFs; n = 11), (iii) alcohol-resistant film-forming fluoroprotein (AR-FFFP; n = 1), and (iv) firefighting foams used for both class A and B fires (AB foam; n = 2). The foams were marketed as organofluorine-containing (n = 14) or as organofluorine-free (n = 10). All products were provided by European manufacturers. na Ten samples of AFFF formulations from seven brands were used in these studies. AFFF formulations were selected from the Department of Defense's qualified product list32 and are assumed to be in active usage; however, individual usage rates for the specific products tested here are not available. 20 L diluted sample na influent water (source waters were river or dam water), ozonation tank effluent, biological activated carbon (BAC) filtration effluent, groundwater treated by hardness reduction, and treated water na Various fluorosurfactants from Shanghei Vatten, China: 3 products that are sold in the domestic market (mainly PFOS based) and 4 alternative products of short chain PFAS-based products that are sold solely in foreign countries na 4 commercially available fluoro products: three fluoro surfactants and an aqueous film-forming firefighting foam 20-500 L household fire estinguisher liquid na 44 soil cores and 17 groundwater samples from fire fighting areas na AFFF samples obtained from U.S. military bases, 3M AFFF from 1988 1 mL diluted sample Nine firefighting foam concentrates: Five concentrates were AR-AFFFPs, two were AR- AFFFs, one was a FFFP and one was fluorine-free (manufactured after 2002) na 62 commercial AFFFs were colleted between 2012 and 2013 in Switzerland and divided into two sets according to the sampling source. A first set was derived from stock solution in fire installation (n = 27) of industrial sites storing chemicals andpetroleum products. A second set was originating from commercially available AFFF between 2012 and 2013 (n = 35) from 6 producers. 500 mg for LC-MS, 200 mg for GC-MS 3 new formulations of AFFFs, branded as Angus- 0.1 mL after fire Tridol, Ansulite, and Angus-fire Tridol oxidation 10 fluorinated AFFF concentrates, 9 of which were obtained from fire sites in Ontario, Canada, and two commercial fluorinated surfactant concentrates na 12 AFFF formulations and 19 groundwater samples obtained from five different military bases within the United States AFFF: 1.5 mL aliquot dilute, Groundwater: 3 mL Archived samples of AFFF formulations manufactured by 3M, Ansul, Chemguard, National Foam, and Buckeye were obtained from U.S. military bases. Groundwater and soil samples were collected in October 2011 from a 1200 m by 600 m area encompassing the burn pit. na 11 AFFF used to extinguish fires in Ontario, Canada, and one commercial product from 3M na 74 QPL-listed AFFF samples with manufacturing dates ranging from 1984 to 2011. Sampling from 21 different US Navy and Air Force military bases within the United States. Sampling instructions specifically stated to sample AFFF from their original product container in order to avoid mixtures of products. FAB: 10:1 with methanol, UPLC/QTOF: 12 ppb, 20 L sample injection size Liquids: method which will provide a representative sample of the liquid to be tested. see sampling FFF samples were provided by the Department of Defence, Australia, including Orchidee (#1), 1 mL sample, diluted Wormald (#2), and in TOP assay reagent Ansulite (#3 and #4) (9 mL) 30 products in 6 different product groups: waterproofing agents, paint, coated fabrics, non- stick ware, electronics and fire fighting agents. They were purchased from retailers in Norway and Sweden. 1 g Pre- treatment Extraction incubated GO membrane in an aqueous solution containing fluorosurfactant (FS), dye and AgNP for an assembly of dye-FS-AgNP-GO na na na 1:93,000 diluted AFFF solution na dilutions with Mili-Q water (10000x for non-targeted, 7500x for TF and IF, 50000x for EOF and targeted) SPE; no extraction for TOP assay UV-based TOP method as faster replacement of conventional heat-based TOP assay, diluted 1000-10,000 SPE according to EPA times Method 537 auto_x0002_mated solid phase extraction (ASPE) na na na 1:1,000 serial dilution of the 3% sample na Sample was mixed to avoid foam formation and were let to rest for a short time period before pipetting and diluting first with deionized water (DI) and then with methanol. A final dilution factor of 100 was obtained for target analysis and for CIC analysis of "organofluorine- free foams" and 10,000 for CIC analysis of organofluorinecontaining foams with a mixture of water:methanol (1:1). For ISE measurement: 20 mL of deionized water, 20 mL of buffer solution, and 100 L of the foam were mixed in a beaker using a stirring bar na AFFF formulations were diluted 100-fold in deionized water. na solid-phase extracted by a concentrator (Waters corporation) through an Oasis WAX cartridge na direct PFAS analysis: sample diluted, pH adjusted to 5-9; TOP assay (total oxidizable precursor): diluted with deionized water (1:10000 on average), potassium persulfate and sodium hydroxide (6 h at 85 C) (PFAA precursors to PFCAs) SPE for not oxidized samples direct sampeling without pre-treatment na diluted 1:100 in methanol na solid phase extraction (SPE) (cartridge Strata X-AW 200mg/6 mL; Phenomenex, France) according to a method previously described (Boiteux et al., 2016) The TOP assay was conducted on aqueous samples using the methods described by Glover et al. (2018). na diluted by a factor of 99 000 in 30% methanol (v/v) in water na diluted in water (5000 to 10 million fold), oxidatiive conversion method to transform PFAA precursors to PFCAs: hydroxyl radicals generated by the thermolysis of only for oxidated persulfate under alkaline pH conditions samples: SPE LC-MS: dissolved in 10 mL water, adding methanol/water, ammonium acetate (pH 4), GC-MS: dissolved in 10 mL methanol, filtration LC-MS: SPE with methanol/ ammonium acetate (50:50) diluted in water, oxidation with KMnO4 and HCl (30 d) na FTICR-MS: diluted between 1000 and 100 000 times Ion Exchange SPE AFFF: diluting into methanol (100,000and 10 million-fold), Groundwater: sonicated AFFF: no extraction, Groundwater: micro- LLE AFFF: two sequential thousand-fold dilutions in methanol, Groundwater: Mixed 1:1 with methanol, dilution Soil: sonification in methanol TOF: diluted 1000-fold with water, LC-MS: diluted by at least 20 000 to 200 000-fold LC-MS/MS: ion-pair method, GC-MS: XAD cartridges diluted to lower concentration with methanol, mixed with 3-NBA for FAB no extraction Dilution for AFFF: Pre-dilute the sample in separate steps with purified water or methanol (1:10 v/v, 1:100 v/v, 1:1 000 v/v) and mix sufficiently (e.g. 500 l sample into 4 500 l diluent). Ensure that there is no phase-separation in the sample. If necessary centrifuge the sample to precipitate non soluble particles. Dilute the pre-diluted sample 1:10 with water or methanol and an appropriate volume of internal standard solution (e.g. 100 l diluted sample, 100 l reference solution, 800 l water or methanol) to have in every dilution (1:10 v/v, 1:100 v/v, 1:1 000 v/v) the same concentration of the internal standard. Transfer an aliquot to a LC vial and analyse the sample. If high PFOS concentrations are expected, begin with the highest dilution (1:10 000 v/v) to avoid a carry over. no extraction 1 mL sample was added into a TOP assay reagent of 9 mL containing 0.066 M of K2S2O8 and 0.15 M of NaOH in a 15 mL centrifuge tube. The mixture was then heated at ~85 C for ~6 h in a temperature-controlled water bath. After the oxidative reaction step, the sample was cooled down to room temperature. The pH of the sample was adjusted to pH 5-9 with concentrated HCl to halt the TOP assay reaction (optimal at pH> 12) and enable the app-based test (optimal at neutral pH). To further halt the reaction, the sample was treated for ~10 min with ultra-sonication. The samples were then stored at 4 C prior to analysis no extraction Liquid and solid samples were homogenized methanol for ionic compounds and ethylacetate for FTOH Clean up After loading, the SERS substrate was washed with water and gently dried with nitrogen blow Measurement surface-enhanced Raman scattering (SERS) Potentiometic detection based on molecular imprinted polymer (MIP), na SEM/EDX A Sciex X500R Quadrupole Time-of- Flight MS (QToF/MS) system using SWATH Data-Independent Acquisition was operated in both positive and negative electrospray ionization (ESI+/-) mode for QToF- na MS and MS/MS analysis. The extracts were blown to dryness using a nitrogen evaporator and reconstituted in 1 mL of LC-MS grade methanol and split between combustion ion chromatography (CIC) and LC-MS/MS. TF/EOF/IF: CIC, TOP assay, LC-MS/MS (targeted), Non-targeted: UPLC with Thermo Orbitrap Fusion mass spectrometer LC-MS/MS, (UPLC, Dionex UltiMate 3000, USA) combined with a tandem triple quadrupole mass spectrometry (MS/MS, AB na SCIEX API 3200, Canada) LC-MSMS The TOP assay was employed to verify a material balance around the precursor compounds. This assay generates hydroxyl radicals by the thermal breakdown of persulfate under basic conditions na (Houtz and Sedlak, 2012). LC-QTOF-MS Acquisition for Soil Analysis LC-MS/MS Acquisition for na Groundwater Analysis UHPLC ( mobile phase consisted of a) 2mM ammonium acetate; and b) 2mM acetonitrile). The XcaliburTM (version4.1; Thermo Fisher Scientific) with Qualbrowser was used for the peak detection, and Compound Discoverer software (version 3.0.0; Thermo Fisher Scientific) with mz Cloud was used for the non-target screening of PFAS na compounds. UPLC-qTOF-ESI-MS (non-targeted), UPLC-MS/MS (targeted), combustion ion chromatograph (CIC) for total fluorine, ion-selective na electrode (ISE) for inorganic fluorine LC-IMS-MS (IMS-QTOF with ESI), MS/MS using a triple, quadrupole na mass spectrometer LC-QToF-MS; SCIEX (Framingham, MA) X500R QTOF system profile analysis with suspect screening against two lists in the NORMAN Suspect List Exchange in firefighting foam impacted environmental and drinking water LC-QTOF-MS in full scan mode na (m/z = 50-1700) na UPLC-MS/MS na ToF-CIMS na LC/IM-QTOF-MS LC-MSMS performance of the analytical method are given in Boiteux et al. (2016)) and TOPA The total oxidizable precursor (TOP) assay was performed ac_x0002_cording to the protocol described by Houtz and Sedlak na (2012)) na LC-qTOF-ESI-MS HPLC-ESI-MS (coupled to QTAP in na case of 6:2 FTAB, 6:2 FtSaAM) LC-MS: adding ammonium hydroxide in methanol (0.5 %), LC- MS/MS, GC-MS/MS for FTOHs, neutralized with acetic acid FTI, FTAC, FTMAC heated, dried, dissolved in water Before and after oxidation: HPLCMS, astk CARE testing kit (visible test of anionic surfactant concentration), ion chromatography, TOF: convert organic fluorine into HF in AQF combustion furnace at 900-1000 C TOF-CIC, QTOF-MS, FTICR-MS, LCMS/MS Groundwater: Methanol added LVI-HPLC-MS/MS Precursor Oxidation Assay with hydroxyl radical (potassium persulfate in NaOH), For soil ENVI-CARB clean-up, neutralized with HCl and amended with methanol LC-MS/MS TOF: convert organic fluorine into HF in AQF combustion furnace at 900-1000 C, TOF-CIC, GC-MS (6:2 FTOH, 6:2 FTSH), LC-MS/MS, 19F NMR na FAB-MS, UPLC/QTOF-MS na LC-qMS, LC-tandemMS no clean-up HPLC-MS/MS and app-based sensor Centrifugation and solvent evaporation, clean up with ENVI-Carb and glacial acetic acid (for ionic PFAS) GC-MS Quantification method no quantification Working range (ng/mMatrices Reported levels (ng/mL) na AFFF na no quantification 10 M - 10 mM AFFF na Internal standardisation using mass- labeled standards and semi-quantification of 63 PFAS through suspect screening analysis na Together, the target analytes and suspect structures are estimated to contribute 129 g/L of fluorine content to the AFFF diluted AFFF. Quantifiying oxidizable precursors using bayesian inference, Internal standardisation using mass-labeled standards for targeted analysis, TF and EOF: Concentrations were determined from the average peak areas of duplicate injections using an eight-point calibration curve of PFOA na isotope-labelled surrogate standards and internal standards na EOF in PFAS-containing AFFF ranged from 220 to 840 mM F, Targeted PFAS explained 1% of AFFF EOF in FT AFFF fluorocarbon surfactants (FSs) PFCA concentrations before and after normal TOP assay were 0-4290 mg L-1 and 438-77,420 mg L-1, respectively. The PFCAs after 60 min UV- based TOP assay was 310-81,881 mg L-1 isotopes na na water and foam na Zwitterionic and cationic compounds composed a majority of the total PFAS mass (up to 97%) in firefighter training area (FTA) soil Perfluorohexane sulfonamide, a potential transformation product of sulfonamide-based PFASs, was present at high concentrations (maximum 448 ng/g in soil, 3.4 mg/L in na soil and water groundwater). 26 PFAS quantified by modified EPA Method 537.1 by Eurofins na PFOS was measured at the highest concentration (9,410 mg/L) followed by AFFF PFHxS (1,500 mg/L) Targeted standardisation using mass- labeled standards, Free inorganic fluoride (IF) was quantified using a fluoride ion- selective electrode (ISE) na Organofluorine surfactants varied between 0.4 and 41.2 mg/L. Among the organofluorine- containing foams, 6:2 FTSA showed a high AFFF relative contribution. no quantification na Targeted: standards na time-aligned in Profinder 8.0 software (Agilent) (Table S2). Suspects were screened against molecular formulas in the NORMAN Suspect List Exchange (Nos. 25, 46), a list of PFASs in the OECD PFASs global database compiled by the U.S. EPA (No. 25, 2019), and a list of PFASs discovered by non-target HRMS na AFFF na AFFF foam contaminated water Long-chain perfluoroalkyl acids (PFAAs) and some of their precursors were specifically found around the firefighting training area The concentration of PFOS in river water was 65-196 ng/L, PFHxS was 88-444 ng/L, PFOA was 0.4-19 ng/L, perfluorohexanoic acid (PFHxA) was 25-78 ng/L internal standardisation using mass- labeled standards na Instrument calibrations na FS, AFFF FS, AFFF Domestic products PFSAs: 0.02-101 g L-1 (mainly PFOS), Alternative products PFASs: ND - 2.1 g L-1 (mainly PFHxS) 6:2 FTOH up to 948 ng L- 1 no quantification household fire extinguisher na liquid na highest total PFAS concentrations (up to 357 mg/g) The highest total PFAS concentrations were recorded in the monitoring wells located in the perimeter of the firefighter training site and in the spring located downgradient in the direction of groundwater flow. They ranged from 300 to 8300 na na soil and water ng/L no quantification na internal standardisation using mass- labeled standards na AFFF na firefighting foam 22500-3188000 g/L internal standardisation using mass- labeled standards na calibration curve using standard solutions of PFOA, PFOS, 6:2FTS, and 8:2FTS na TOF-CIC: external calibration, no quantification for MS na AFFF PFOS Median: 635 mg/kg 6:2 FTS up to 1010 ppm (mg/L) after oxidation, no AFFF PFOS AFFF TOF: up to 55 g of F internal standardisation using mass- labeled standards na AFFF, groundwater AFFF: up to 550 ng/L for PFPeSaAm, Groundwater: up to 6900 ng/L for 6:2 FtTAoS, 360,000 for PFHxS isotope dilution with isotopically labeel standards, fluorotelomer precursors with C6 homologue, estimation for no standard avaliable na AFFF, groundwater, soil AFFF: oxidation of PFAA generate 5.9 - 10.8 g/L carboxylates, Groundwater: PFOS = 19 g/L, PFOA = 26 g/L, PFHXS = 71 g/L, PFHxA = 36 g/L; Soil: PFOS = 2400 g/kg, PFHxS = 66 g/kg TOF: conductivity detector, LC-MS: PFCAs/ FTUCAs: internally calibrated using corresponding mass-labelled standards (PFOS, PFDoDA), 6:2 FTSA/6:2 FTSAS: External calibration na TOF: 475 to 18 000 g F mL-1, 6:2 FTSAS > 1000 AFFF g mL-1 no quantification AFFF not reported Quantify the samples by using the unextracted external calibration curve. When spiking with labelled reference solutions, the determination of the concentration is independent of possible errors made during injection. Also, errors caused by sample losses during distinct steps of sample pre-treatment or the adjustment of final sample extract volume as well as matrix effects in the sample are accounted for. Method is applicable for a concentration range for PFOS in the extract solution of 0,5 g/l to 50 g/l. Coated materials like paper, textile, leather, carpets, clothes and footwear, Non-coated materials, liquids na Quantification was performed by producing a calibration curve using standard solutions (external) of PFOA and PFOS (only linear isomers) with correlation coefficients higher than 0.99. internal standard na AFFF range 10 - 500 g/L food contact paper, textile, fire fighting foam, water proofing agents and lubricants, paint, leather, carpets, nonstick ware, printed circuit boards info - validation of the method na Limitations na na na na na Recoveries for each targeted PFAS 77 ranged from The availability of analytical standards has 72-130%, except for 8:2 FTSA (62%) and 10:2 FTSA not kept pace with the new PFAS in (45%), TF: Relative standard deviations of commerce, and the existence of chemical duplicate injections <8% and method recovery standards does not always 99%, EOF: relative standard deiations <5%, immediately result in the expansion of method recovery 96% common PFAS testing panels. na na recovery: 14-23% RSD 95% na na na na na several quality control tests, replicate, blank samples,... Robustness: two different chromatographic analyses gave comparable mass spectra na na na na na na na strictly following the quality assurance and quality control procedure na na na na na na na na na na na na results from 2 laboratories were consistent na na na na na na relative standard deviations for the same sample analysed on different days were less than 10%for total fluorine and less than 5% for inorganic fluorine na A limitation of the FAB-MS/QTOF-MS method is that it can only capture the major components and that minor (approximately <0.1%) fluorochemical compounds may go undetected The recovery of labelled reference compound shall be in the range from 70 % to 125 % for the sample to be considered valid. The dilution error introduced by this method should be much smaller than the analytical error involved in the method. As a general rule the dilution error should be less than 1 %. na For quality assurance and quality control (QA/QC), at least three samples were run in parallel for each test including one for the ``Before'', one for the ``Control'' and one for the ``After'' sample. Moreover, TOP assay results using HPLC presented in this work were also validated with assistance from ALS Global, to compare with the results in our laboratory, including using HPLC and app-based sensors. Laboratory duplicate, method blank, laboratory control spike and matrix spike were generally conducted to monitor the test recovery and the acceptance limits The possible reasons for the variations: (i) further oxidation might release an ultrashort chain of PFAS that currently cannot be quantitatively monitored; (ii) incomplete oxidation of PFAS precursors due to the presence of organic matter; (iii) the random nature of TOP assay oxidation that can be affected by many parameters, including the TOP assay reagent amount and the initial concentration of PFAS. As standard procedure, laboratory blanks, method detection limits (MDLs) and recoveries were examined. For each sample, a high resolution full scan spectra was used to control positive detections (typical mass tolerance 50 ppm). No laboratory contamination for any of the analyzed compound was detected na LoD (ng/mL) subgroup ~50 ppb (~120 nM for PFOA) Measurement - generic name SERS down to 100 nM (~41 ppb for PFOA) sensor (MIP, SEM/EDX) not reported LC-HRMS Targeted: MDL = 2.7838,86, 116.92 (PFTeDA), 131.88 (PFNS) nM F CIC, TOP assay, LC-HRMS na na LC-MS/MS na LC-MS/MS na LC-HRMS MDL= 6750-250000 ng/ L LC-MS/MS Targeted: MDL = 1-2 g/L, CIC: MDL = 0.2 m/ L, ISE: MDL = 800 g/L LC-HRMS not reported SI (no access) LC-HRMS (with ion mobility) LC-HRMS na LC-HRMS LOD = 0.09-0.60 ng mL1, LOQ = 0.11-1.79 ng mL-1 detection limit: 1.4-7.9 pptv LC-HRMS LC-HRMS not reported LC-HRMS na LC-MS/MS not reported LOQ = 5000 g/L for targeted PFASs LC-MS/MS LC-HRMS LOQ: 0.5-2 ng/mL (LCMS), 2-10 ng/mL (GCMS) LOD ~0.2 ppm, astkCARE testing kit: LOD = 0.1 ppm not reported LC-MS, GC-MS LC-MS/MS LC-HRMS, LC-HRMS Median LOD = 1.7 ng/L (0.71 ng/L for PFDS - 67 ng/L for 6-2 FtSaAm), LOQ = 2.4 - 221 ng/L LC-MS/MS Soil preparation: LOD = 0.4 to 3 g/kg, Groundwater preparation: LOD = 0.1 to 0.5 g/L LC-MS/MS LOQ = 0.05 - 1 g/mL, 1 g/mL for 6:2 FTCA, 5:3 FTCA, other analytes < 0.2 g/mL FAB-MS analysis has poor sensitivity (approximately mg/L levels) CIC, GC-MS, LC-MS/Ms, 19F NMR FAB-MS, LC-HRMS na LC-MS/MS HPLC-MS/MS and appbased sensor in the range of 10 - 500 g/L LC-MS/MS, sensor MDLs not reported na GC-MS Title Per- and polyfluoroalkyl substances in serum and associations with food consumption and use of personal care products in the Norwegian biomonitoring study from the EU project EuroMix Automated online solid-phase extraction liquid chromatography tandem mass spectrometry investigation for simultaneous quantification of per- and polyfluoroalkyl substances, pharmaceuticals and personal care products, and organophosphorus flame retardants in environmental waters Per- and polyfluoroalkyl substances and fluorine mass balance in cosmetic products from the Swedish market: implications for environmental emissions and human exposure Fluorinated Compounds in North American Cosmetics Correction to "Fluorinated Compounds in North American Cosmetics" Occurrence of perfluorinated carboxylic acids (PFCAs) in personal care products and compounding agents Faktablad - PFAS i kosmetiska produkter Risk assessment of fluorinated substances in cosmetic products Authors Journal year Thepaut et al. Environmental Research 2021 Vol. 195 2021 Zhong et al. Journal of Chromatography A 2019 Vol. 1602 Pages 350-358 2019 Schultes et al. Environmental Science-Processes & Impacts 2018 Vol. 20 Issue 12 Pages 1680-1690 2018 Whitehead et al. Environ. Sci. Technol. Lett. 2021, 8, 538-544 2021 Whitehead et al. Yukiko Fujii et al. Environ. Sci. Technol. Lett. 2021, 8, 1104-1105 Chemosphere 2021 2013 Naturskyddsfreningen (Nature Conservation Association) na na The Danish Environmental Protection Agency na 20018 comments (t, nt, o) DOI link na 10.1016/j.envres.2021.110795 na 10.1016/j.chroma.2019.06.012 na 10.1039/c8em00368h na 10.1021/acs.estlett.1c00240 Due to a calibration problem with the targeted analysis affecting only the Canadian products (n = 17), in our original article (https://pubs.acs.org/doi/10.1021/ acs.estlett 1c00240), data for Canadian products were requantified using the isotopically labeled surrogate standards https://pubs.acs.org/doi/10.1021/acs. 10.1016/j.chemosphere.2013.06.04 na https:// old.naturskyddsforeningen.se/sites/ default/files/dokument-media/ na bilaga_press_och_webb.pdf na https://www2.mst.dk/Udgiv/publication PFAS 6:2PAP, 8:2PAP, 6:2diPAP, 8:2diPAP, PFHxPA, PFOPA, PFDPA, PFBS, PFHxS, PFHpS, PFOS, PFDS, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFOSA, MeFOSA and EtFOSA perfluorobutanoic acid (PFBA); perfluoropentanoic acid (PFPeA); perfluorohexanoic acid (PFHxA); perfluoroheptanoic acid (PFHpA); perfluorooctanoate (PFOA); perfluorononanoic acid (PFNA); perfluorodecanoic acid (PFDA); perfluoroundecanoic acid (PFUnDA); perfluorododecanoic acid (PFDoDA); perfluorotridecanoic acid (PFTrDA); perfluorobutanesulfonate (PFBS); perfluoropentanesulfonate (PFPeS); perfluorohexanesulfonate (PFHxS); perfluoroheptanesulfonate (PFHpS); perfluorooctanesulfonate (PFOS) perfluorodecanesulfonate (PFDS); 4:2 fluorotelomer sulfonic acid (4:2 FTS); 6:2 fluorotelomer sulfonic acid (6:2 FTS); 8:2 fluorotelomer sulfonic acid (8:2 FTS); N_x0002_ethylperfluorooctanesulfonamide (EtFOSA); Nmethylperfluorooctanesulfonamide (MeFOSA); chlorinated polyfluorinated ether sulfonate (6:2F-53B); linear isomers of PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFHxS, PFOS, FOSA, 6:2 FTSA, 6:2 monoPAP, 8:2 monoPAP, 6:2/6:2 diPAP and 8:2/8:2 diPAP. Level 2 was given to the following 13 targets for which a native standard was available but not an exactly matched isotopically labelled standard: PFTrDA, ADONA, 9Cl-PF3ONS, 11Cl-PF3OUdS, PFBS, PFDS, FOSAA, 4:2 FTSA, 8:2 FTSA, 4:2 monoPAP, 10:2 monoPAP, 4:2/4:2 diPAP and 6:2/8:2 diPAP. Total fluorine, Targeted analsis of PFPrA, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFHxDA, GenX, PFPrS, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFECHS, Cl-PFOS, 6:2 FTCA, 8:2 FTCA, 4:2 FTSA, 6:2 FTSA, 8:2 FTSA, 6:2 Cl-PFESA, 8:2 ClPFESA, FBSA, FHxSA, FOSA, MeFOSA, EtFOSA, 6:2 PAP, 8:2 PAP, 6:2 diPAP, 6:2/8:2 diPAP, 8:2 diPAP, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, MeFOSE, EtFOSE, 6:2 FTAc, 8:2 FTAc, 10:2 FTAc, 6:2 FTMAc, 8:2 FTMAc na Target PFAS included PFHxA,PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA 16 different PFAS were analysed: (PFBS, PFHxS, PFOS, PFDS, PFOSA, 6:2 FTS, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTriDA, PFTeDA, and PFHxDA TOF and targeted analysis of Perfluorobutanoic acid (PFBA) Perfluoropentanoic acid (PFPeA) Perfluorohexanoic acid (PFHxA) Perfluoroheptanoic acid (PFHpA) Perfluorooctanoic acid (PFOA) Perfluorononanoic acid (PFNA) Perfluorodecanoic acid (PFDA) Perfluoroundecanoic acid (PFUnA) Perfluorododecane acid (PFDoA)Perfluorotridecanoic acid (PFTrA) Perfluorotetradecanoic acid (PFTeA) Perfluoro-3,7-dimethyloctanoic acid (PF-3,7-DMOA) 7H-Dodecafluoroheptanoic acid (HPFHpA) Perfluorobutane sulfonate (PFBS) Perfluorohexane sulfonate (PFHxS) Perfluoroheptane sulfonate (PFHpS) Perfluorooctane sulfonate (PFOS) Perfluorooctane sulfonamide (PFOSA) Perfluorodecane sulfonate (PFDS) 4:2 Fluorotelomer sulfonate (4:2 FTS) 6:2 Fluorotelomer sulfonate (6:2 FTS) 8:2 Fluorotelomer sulfonate (8:2 FTS CAS (if available in source) na na na na na na na na Sampling sample amount used Participants (44 males and 100 females) kept detailed diaries on their food consumption and their PCP use for two non-consecutive days. All urine (24 h) and blood samples were collected at the end of each study day 50 L of blood na na thirty-one CPs from five product categories (cream, foundation, pencil, powder and shaving foam) 0.1 g for LC-MS (injected (5 l)), 100 l sample extracts for TF/EOF, 5 mg of neat CP material for TF analysis and 0.05-0.8 g of CP material for EOF depending on the expected fluorine concentration. 231 cosmetic products, 29 for targeted analysis 50-100 mg for targeted analysis na na 16 commercially available cosmetic samples and 10 sunscreen products distributed by eight different companies. In addition to these end consumer products, we also obtained commercially available compounding agents, including mica and talc, which 1-200 mg depending on the were treated with PAPs. PFCA concentration 22 cosmetic products from nine different brands, The products come from well-known brands and were randomly selected. All products had declared contents of fluorine. na 18 products that had declared content of the selected PFAS 0.1 g for LC-MS, 1 g for TOF Pre- treatment na An automated Agilent 1260 Infinity Flexible Cube was employed to achieve online preconcentration of all analytes LC-MS: samples vortexed used without homogenizing the entire mass or volume na na na homogenised, tablets pressed for TOF Extraction Clean up na na na na LC-MS: sonication in methanol/NaOH (method adapted from Powley et al. (2005)) LC-MS: concentrated, Supelclean ENVI-carb. Before injection, the samples were vortexed, centrifuged and transferred to a micro vial. targeted analysis: sonicating Targeted analysis: Envi-Carb twice with 4:1 hexane- for cleanup, concentrated isopropanol and twice with again under nitrogen, and 1:1 methanol-acetonitrile filtered na na ion-pair extraction No further clean-up was conducted na na LC-MS: sonification with methanol, no extraction for TOF LC-MS: activated carbon was added to the sample extract to eliminate interfering sample matrix components, some additionally purified by solidphase extraction (SPE) Measurement a high throughput online solid phase extraction ultra-high_x0002_performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method as described by Poothong et al. (2017a) An Agilent 1260 series RPLC was used to perform chromatographic analyses. The analytical separation was achieved using an Agilent Poroshell 120EC-C18 (3.0 50 mm, 2.7 m) column maintained at 30 C. A delay column (Agilent Eclipse Plus C18, 4.6 50 mm, 5.0 m) was installed after the mixing valve of the binary pump. The second valve was switched at 4 min. For chromatographic elution, the mobile phase was composed of acetonitrile (ACN) and water with 0.05% formic acid, and the flow rate was 0.30 mL min-1 . The gradient elution profile was programmed as follows: 0-4 min, 5% ACN; 4-9 min, 5-60% ACN; 9-16 min, 60-100% ACN; and, 16-21 min, 100% ACN. A 9 min re-equilibration period was included before the next analysis, resulting in an overall method run time of 30 min An Agilent 6470 triple quadruple mass spectrometer with a Jet Stream electrospray ionization (ESI) source was operated under dynamic multiple reaction monitoring (DMRM) mode with a retention time (RT) window of 1-2 min. liquid chromatography_x0002_tandem mass spectrometry, as well as extractable organic fluorine (EOF) and total fluorine (TF) by combustion ion chromatography (CIC) Extracts were injected (5 ml) onto an Acquity UPLC (Waters Corp., Milford, MA) equipped with BEH C18 guard (5 _x0003_ 2.1 mm, 1.7 mm particle size) and analytical (50 _x0003_ 2.1 mm, 1.7 mm) column operated at 40 _x0004_C. Detection of PFASs was carried out using a triple quadrupole mass spectrometer (Xevo TQ-S, Waters Corp, Mil_x0002_ford, MA) operated in negative electrospray ionization mode according to a method reported by Gebbink et al TF and EOF measurements were carried out at SU using a Thermo-Mitsubishi combustion ion chromatograph (CIC). Sample extracts (100 ml) were placed in a ceramic sample boat containing glass wool for better dispersion of the uids while neat CP material was weighed directly into the sample boat. All boats were baked prior to sample combustion to minimize background contamination. The samples were combusted slowly in a combustion furnace (HF-210, Mitsubishi) at 1100 _x0004_C under a ow of oxygen (400 l min_x0001_1 ) and argon mixed with water vapor (200 l min_x0001_1 ) for approximately 5 minutes. Combustion gases were absorbed in MilliQ water during the entire length of the combustion process using a gas absorber unit (GA-210, Mitsubishi). An aliquot of the absorption solution (18 or 200 ml, depending on sample concentration) was injected onto an This journal is The Royal Society of Chemistry 2018 Environ. Sci.: Processes Impacts, 2018, 20, 1680-1690 | 1683 Paper Environmental Science: Processes & Impacts Open Access Article. Published on 01 November 2018. Downloaded on 1/21/2019 4:25:52 AM. This article is licensed under a Creative Commons Attribution-NonCommercial 3.0 Unported Licence. View Article Online ion chromatograph (Dionex Integrion HPIC, Thermo Fisher Scientic) equipped with an anion exchange column (Dionex IonPac AS19 2 _x0003_ 50 mm guard column and 2 _x0003_ 250 mm analytical column, 7.5 mm particle size) operated at 30 _x0004_C. total fluorine using PIGE, targeted LC-MS/MS and GC-MS total fluorine using PIGE, targeted LC-MS/MS and GC-MS GC/ECNI/MS in selected ion monitoring mode (Agilent 6890GC/5973MSD inert, Agilent Technologies Japan, Ltd., Tokyo, Japan) LC/HRMS-MS LC-MS/MS, IC for TOF Quantification method Working range (ng/mMatrices Multivariable linear regressions were performed between each food and PCP category and each chemical and were sex_x0002_stratified when the consumption of food or use of PCPs was significantly different between men and women. na serum and urine drinking water, surface na na water and waste water Quantification of TF and EOF was carried out using a linear six-point calibration curve of PFOS ranging from 0.5 to 100 g ml-1 0.5 to 100 g ml-1 moisturizing creams (abbreviated CRE), founda_x0002_tions (FOUN), powders and eye shadows (POW), eye pencil (PEN) and shaving foams (SHAV) surrogate standards na various cosmetic samples isotopically labeled surrogate standards na internal mass-labeled standards and external calibration standards na foundation, lip, mascara cosmetic samples (Manicure, (powder) foundation, Lip rouge), suncream samples na na cosmetic samples internal standards for LC-MS na cosmetic samples reported levels (ng/mL) info - validation of the method PFHxS, PFHpS, PFOS, PFDS, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, and 6:2diPAP were detected in 75-100% of the serum samples. PFHxPA, 8:2diPAP, PFHxA, PFOSA, and PFBF were detected in 52-68% of the serum samples, while MeFOSA, 8:2PAP, 6:2PAP, PFPeA, and PFTeDA were detected in 3-29% of the samples. Some chemicals (PFOPA, PFDPA, PFHxA and EtFOSA) were below the LOD in all serum samples On average, they were found at 5.7, 1.7, 0.9, and 0.8 ng/mL in females and 9.3, 2.1, 1.3, and 1.1 The accuracy of the method ranged between 90% ng/mL in males and 114% six other PFAS (e.g., PFBS, PFHxA, PFOA, PFOS, PFNA, and PFUnDA) were detected in surface water at concentration below 18 ng L-1 . PFOAwas the only PFAS detected in the DWTP influent. Besides the six PFAS mentioned above, PFPeA, PFHpA, PFDA, and 6:2 F-53B were also detected in WWE at concentrations ranging from 2 to 48 ng L1 accuracy with 82% of analytes exhibiting 70-130% recovery linearity (R2 was higher than 0.984 Analyte recovery and intra-day precision were evaluated in triplicate Recovery was determined by comparing the concentration measured by the online SPE-LC-MS/MS method, calculated using the calibration curve for ultrapure water (above), with the initial spiking levels. recoveries of 70-130%. The intra-day precision of each analyte at the three spiking levels was evaluated as the relative standard deviation (RSD) of the replicate measurements. The inter-day precision was reported for each matrix as the RSD of 15 replicates magnitude of MEs on ESI for some analytes Foundations and powders contained 25 different PFASs with the most frequently detected being perfluorinated carboxylic acids (perfluoroheptanoic acid and perfluorohexanoic acid) and polyfluoroalkyl phosphate esters (PAPs). S14PAP concentrations up to 470 mg g_x0001_1 creams, pencil and shaving foams did not contain measurable concentrations of any of the 39 PFASs targeted. The highest TF concentrations were found in powders (547-19 200 mg g_x0001_1 ), closely followed by creams (<LOD - 11 100 mg g_x0001_1 ) and foundations (326-3120 mg g_x0001_1 ). PFASs measured by LC-MS/MS, triplicate spike/ recovery experiments were performed by fortifying a PFAS-free cosmetic (FOUN07) at two fortication levels Method accuracy, as assessed through spike/recovery experi_x0002_ments, ranged from 71 to 126% for most PFASs Results of the inter-laboratory comparison on a subset of 18 samples (unfortied) revealed good agreement between labs, with a coefficient of determination of 0.9605 for 11 targeted PFAS measuremen foundations, mascaras, and lip products had the highest proportion of products with high total fluorine 0.384 g F/cm2 PFAS concentrations ranged from 22-10,500 ng/g product weight matrix spike recoveries of individual analytes were all within 80%-115% foundations, mascaras, and lip products had the highest proportion of products with high total fluorine 0.466 g F/cm2 PFAS concentrations ranged from 0.23-10,500 ng/g product weight na The maximum concentrations of total PFCAs were 5.9 g g-1 for cosmetics and 19 g g-1 for sunscreens. total analyte recoveries ranging from 60% to 83% Total PFAS from 0.13 ng/g to 7,730 ng/g na The highest concentration of a single substance was 3,340 ng/g PFHxA, There was a relatively large difference between the content of the individual PFAS and the concentration of organic fluorine in the products. na Limitations LoD (ng/mL) subgroup 0.002 ng/mL and 0.090 na ng/mL Cosmetics The method detection limits (MDLs) ranged na from 0.16 to 5.13 ng L-1 na some of the listed fluorinated ingredients (e.g. fluorinated silanes, polymeric substances) were not quantified due to the TF: LOD = 91.1 g g-1, lack of MS-based methods EOF: LOD = 1.02 to 6.65 and/or authentic standards g g-1 na LOD (PIGE): 0.127 g F/cm2, MDLs ranged from 0.01 ng/g for PFPeS to 12.0 ng/g for 8:2 FTOH na 0,05 ng/g na na na na MDL = 0.7 (PFTeDA) - 66 concentrations of PAPs were (PFHxA) ng g-1, MQL = not determined 2.3 - 176 ng g-1 na na na na na na na Measurement - generic name LC-MS/LMS LC-MS/LMS LC-MS/LMS, CIC LC-MS/MS, GC-MS PIGE, LC-MS/MS, GC-MS GC-MS LC-HRMS LC-MS/MS, CIC Title Authors Effects of outdoor weathering and laundering on the detection and classification of fluorinated oil-and-water-repellent fabric coatings Dolan et al. Detection and diversity of fluorinated oil- and waterrepellent coatings on apparel fibers Dolan et al. Hydrolysis of FTOH precursors, a simple method to account for some of the unknown PFAS Nikiforov et al. Journal year Journal of Forensic Science Journal of Forensic Science 2021 2021 Chemosphere 2021 Combined use of total fluorine and oxidative fingerprinting for quantitative determination of side-chain fluorinated polymers in textiles Liagkouridis et al. Post-Chromatographic Dicationic Ionic Liquid-Based Charge Complexation for Highly Sensitive Analysis of Anionic Compounds by Ultra-High- Performance Supercritical Fluid Chromatography Coupled with Electrospray Ionization Mass Spectrometry Li et al. Analytical Chemistry 2021 Anal Chem 2021 Side-chain fluorotelomer-based polymers in children car seats Wu et al. Environmental Pollution 2021 Solid phase extraction of perand polyfluoroalkyl substances (PFAS) from clothing Machery-Nagel Application Notes 2020 The effect of weathering on per- and polyfluoroalkyl substances (PFASs) from durable water repellent (DWR) clothing Van der Veen et al. Selective and sensitive analysis by reactive easy ambient sonicspray ionization: Synergistic combination of non-polar spray solvent and dicationic ionic liquid Lv et al. Elemental Fluorine Detection by Dielectric Barrier Discharge Coupled to Nano electrospray Ionization Mass Spectrometry for Nontargeted Analysis of Fluorinated Compounds Zheng et al. Chemosphere 2020 Talanta 2020 Analytical Chemistry 2020 Another Pathway for Firefighter Exposure to Per- and Polyfluoroalkyl Substances: Firefighter Textiles Peaslee et al. Environmental Science & Technology letters 2020 Total oxidizable precursor assay in the determination of perfluoroalkyl acids in textiles collected from the United States Zhu et al. Elsevier 2020 Derivatization of Perfluorocarboxylic Acids with N,N-Dimethylformamide Dimethylacetal Prior to GC-MS Analysis Strozynska et al. Rapid analysis of perfluorinated carboxylic acids in textiles by dielectric barrier discharge ionization-mass spectrometry Wang et al. Chromatographia 2020 Vol. 83 Issue 3 Pages 477-482 2020 Microchemical Journal 2020 Vol. 155 2020 How Do We Measure Poly- and Perfluoroalkyl Substances (PFASs) at the Surface of Consumer Products? Tokranov et al. Release of Side-Chain Fluorinated Polymer-Containing Microplastic Fibers from Functional Textiles During Washing and First Estimates of Perfluoroalkyl Acid Emissions Schellenberger et al. Environ Sci Technol Lett 2019 Environmental science & Technology 2019 Survey of perfluorinated compounds in consumer products by liquid chromatography-tandem mass spectrometry Lee et al. Energy & Environment 2020 Vol. 31 Issue 4 Pages 713-729 2019 Classifying single fibers based on fluorinated surface treatments Dolan et al. Previously unidentified sources of perfluoroalkyland polyfluoroalkyl substances from building materials and industrial fabrics Janousek et al. Analytical and Bioanalytical Chemistry volume 2019 Environmental Science Processes & Impact 2019 Per- and polyfluorinated compounds in saleswomen's urine linked to indoor dust in clothing shops Wu et al. ISO 23702-1:2018 - Leather -- Organic fluorine -- Part 1: Determination of the nonvolatile compound content by extraction method using liquid chromatography/ tandem mass spectrometry detector (LC-MS/ MS) Science of the Total Environment 2019 2018 Development of Extraction Methods for the Analysis of Perfluorinated Compounds in Leather with High Performance Liquid Chromatography Tandem Mass Spectrometry Zhang et al. 5th Annual International Conference on Material Science and Environmental Engineering, edited by K. Wang 2018 Closing the Mass Balance on Fluorine on Papers and Textiles Robel et al. Environ Sci Technol 2017 Analysis of PFASs and TOF in products Nordic Council of Daniel Borg, Jenny Ivarsson Ministers PIGE as a screening tool for Per- and polyfluorinated substances in papers and textiles Ritter et al. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 2017 2017 In-Vial Extraction Large Volume Gas Chromatography Mass Spectrometry for Analysis of Volatile PFASs on Papers and Textiles Rewerts et al. Development and validation of a method for the quantification ofextractable perfluoroalkyl acids (PFAAs) and perfluorooctanesulfonamide (FOSA) in textiles Van der Veen et al. Environ Sci Technol 2017 Talanta 2016 Screening for perfluoroalkyl acids in consumer products, building materials and wastes Becanova et al. Systematic determination of perfluoroalkyl and polyfluoroalkyl substances (PFASs) in outdoor jackets Gremmel et al. Perfluorooctane sulfonate (PFOS) andperfluorooctanoic acid (PFOA) contamination from textiles Supreeyasunthron et al. Chemosphere Chemosphere Journal of Environmental Science and health, Part A 2016 2016 2016 Polyfluoroalkyl substances (PFASs) in textiles for children The Danish Environmental Protection Agency 2015 Rapid fluorometric determination of perfluorooctanoic acid by its quenching effect on the fluorescence of quantum dots Liu et al. journal of Luminescense 2015 Analysis of per- and polyfluorinated substances in articles Blom et al Rapid screening and identification of multi-class substances of very high concern in textiles using liquid chromatography-hybrid linear ion trap orbitrap masss pectrometry Zhang et al. Nordic Council of Ministers 2015 Journal of Chromatography A 2015 Perfluoroalkyl and polyfluoroalkyl substances in consumer products Kotthoff et al. Determination of fluorotelomer alcohols in selected consumer products and preliminary investigation of their fate in the indoor environment Liu et al. Environ Sci Pollut Res Int 2015 Chemosphere 2015 Are imported consumer products an important diffuse source of PFASs to the Norwegian environment? Vestergren et al Environmental Pollution 2015 Concentrations and trends of perfluorinated chemicals in potential indoor sources from 2007 through 2011 in the US Liu et al. Chemosphere 2014 Understanding the exposure pathways of per- and polyfluoralkyl substances (PFASs) via use of PFASs-containing products - risk estimation for man and environment UMWELTBUNDESAMT 2014 Detection of fluorotelomer alcohols in indoor environments and theirrelevance for human exposure Schlummer et al. Removing perfluorooctane sulfonate and perfluorooctanoic acid from solid matrices, paper, fabrics, and sand by mineral acid suppression and supercritical carbon dioxide extraction Chen et al. Environmental International Chemosphere 2013 2012 Perfluoroalkyl and polyfluoroalkyl substances (PFASs) in consumer productsin Norway - A pilot study Herzke et el. Chemistry for any weather Greenpeace CEN/TS 15968:2010 Determination of extractable perfluorooctanesulphonate (PFOS) in coated and impregnated solid articles, liquids and fire fighting foams - Method for sampling, extraction and analysis by LCqMS or LC-tandem/MS Chemosphere 2012 2012 2010 Combined Use of Total Fluorine and Oxidative Fingerprinting for Quantitative Determination of Side-Chain Fluorinated Polymers in Textiles Liagkouridis et al. Environmental Science and technology 2022 DIN EN 17681-1 Textiles and textile products - Organic fluorine. Part 1: Determination of non-volatile compounds by extraction method using liquid chromatography. DIN EN 17681-2 - Textiles and textile products - Organic fluorine - Part 2: Determination of volatile compounds by extraction method using gas chromatography 2021 Draft Edition 2021-07 Comments DOI link Effects of weather and laundering were tested by pyrolysis pyrolysis were used https://doi.org/ Test was done to find our what kind of PFAS 10.1016/ you actually find when you do a TOF- j.chemosphere.2021. analyses 130044 This content is an early or alternative research output and has not been peer- 10.33774/chemrxiv- reviewed at the time of posting. 2021-jpxbh 10.1021/ acs.analchem.0c046 12 https://doi.org/10.101 basis of the methodology of DIN 38407-42 https://www.mn- net.com/media/pdf/ 3e/87/76/AN-072020-SPE-of-PFASfrom-clothing-EN.pdf Increase of detected PFAS after weathering https://doi.org/ 10.1016/ j.chemosphere.2020. 126100 Method development with PFOA, PFOS as model analyts 10.1016/ j.talanta.2020.12092 9 novel atmospheric-pressure elemental ionization method where fluorinated compounds separated by gas chromatography (GC) are converted to Na(2)F(+) for nontargeted detection https://dx.doi.org/10. https://dx.doi.org/10. https://doi.org/ 10.1016/ j.envpol.2020.11494 0 10.1007/s10337019-03850-6 10.1016/ j.microc.2020.10477 3 Method development for consumer products 10.1021/ acs.estlett.8b00600 The amount of released fibres is the primary 10.1021/ topic of this article acs.est.9b04165 10.1177/0958305x1 9882376 10.1007/s00216019-01596-6 10.1039/ c9em00091g https://doi.org/ 10.1016/ j.scitotenv.2019.02.2 87 https://www.restek.com/en/technical-literatu 10.1088/1757-899x/ 301/1/012046 Mass balance between PIGE and other methods 10.1021/ acs.est.7b02080 http://dx.doi.org/10.6 https://doi.org/10.101 Development of method 10.1021/ acs.est.8b04304 http://dx.doi.org/ 10.1016/ j.talanta.2015.09.02 1 10.1016/ j.chemosphere.2016. 08.1120045-6535/ 10.1016/ j.chemosphere.2016. 06.043 0045-6535/ http:// dx.doi.org/ 10.1080/10934529. 2015.1128713 Also migration of PFASs to saliva and washing investigated https://www2.mst.dk/ Method improvement 10.1016/ j.jlumin.2015.01.045 0022-2313/ na http://dx.doi.org/10.6 http://dx.doi.org/ New analytical method was established and 10.1016/ validated for the analysis of 19 substances of j.chroma.2015.01.07 very high concern (SVHCs) in textiles 7 10.1007/s11356015-4202-7 10.1016/ j.chemosphere.2014. 06.012 10.1016/ j.envpol.2014.12.034 10.1016/ j.chemosphere.2013. 10.001 https:// www.umweltbundes amt.de/en/ publikationen/ understanding-theexposure-pathwaysof-per Method development: 10.1016/ j.envint.2013.03.010 10.1016/ j.chemosphere.2012. 06.003 10.1016/ j.chemosphere.2012. 03.035 https://www.greenpe Also used for other matrices, sample treatmant different https://pubs.acs.org/d Method includes not only the standard PFAS but also others; MeFOSE, EtFOSE, 4:2-FTOH, 6:2-FTOH, 8:2-FTOH, 10-2 FTOH and PF-3,7DMOA, 7HPHpA, 4HPFUnA and HPFO-DA-X (acyl halides). Stability: The stability of PFAS in methanol is 6 months, but the stability of PFAS in methanol/water is only 1-2 days, especially for the FTOH substances. Therefore, a dilution on a working day basis is necessary PFAS CAS (if available in publication) Fluorine from fluorinated pyrolysis products na Fluorinated pyrolysis products na FTOH polymers na total fluorine, Side-chain fluorinated polymers (SFPs) after TOP assay as PFAAs na PFDoA, PFUdA, PFDA, PFNA, PFOA, PFHpA, PFHxA, PFPeA, PFOS, PFBS na 12 PFCAs (including PFOA) 8 PFSA's (including PFOS) 3 fluorotelomer acids 12 neutral PFAS na 40 PFAS: 3,6-OPFHpA, PFBA, PF4OPeA, PFPeA, PF5OHxA, FBSA, L-PFBS, PFHxA, PFEESA, 4:2FTS, HFPO-DA, L-PFPeS, PFHpA, NaDONA, FHEA, FHxSA, PFHxSK, PFOA, 6:2FTS, L-PFHpS, PFNA, FOEA, FOSA, PFOSK, PFDA, 8:2FTS, 9Cl-PF3ONS, LPFNS, PFUdA, N-MeFOSAA, FDEA, N-EtFOSAA, LPFDS, PFDoA, 11Cl-PF3OUdS, PFTrDA, PFTeDA, 6- 2diPAP, 628-2diPAP, 8-2diPAP, MPFBA, M5PFPeA, M3PFBS, M5PFHxA, M2-4FTS, M4PFHpA, MFHEA, M3PFHxS, M8PFOA, M2- 6:2FTS, M9PFNA, MFOEA, M8FOSA, M8PFOS, M6PFDA, M2-8:2FTS, M7PFUdA, d3-N-MeFOSAA, MFDEA, d5-N-EtFOSAA, MPFDoA, M2PFTeDA na PFBA, PFPeA, PFHxA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, L-PFBS, L-PFHxS, L- PFHpS, L-PFOS, FOSA, 4:2 FTSA, 6:2 FTSA, 8:2 FTSA, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 6:2 FTAC, 8:2 FTAC, 10:2 FTAC, 6:2 FTMAC, 8:2 FTMAC, 10:2 FTMAC, na PFOA, PFOS na nontargeted detection, good efficiency regardless of the chemical structure na Total fluorine, Targeted analysis of PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFBS, PFOS, 6:2 FTS, 8:2 FTS na PFBS, PFHxS, PFOS, PFDS, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, precursors (TOP assay) na perfuorocarboxylic acids (PFCA, C4-C12) na PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA na surficial fluorine content, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFBS, PFHxS, PFOS, FOSA, 6:2 FtS, N-MeFOSAA, N- EtFOSAA na total fluorine na PFHXA, PFHpA, PFOA, PFNA, PFDA, PFBS, PFHxS, PFOS, PFOSA, N-MeFOSA, N-EtFOSO 307-24-4, 375-85-9, 335-67-1, 375-95-1, 335-76-2, 375-73-5, 355-46-4, 1763-23-1, 754-91-6, 31506-32-8, 4151-50-2 Fluorine from fluorinated pyrolysis products PFCAs (C4-C14), PFSAs (C4-C8,C10 and C12),n:2 fuorotelomer sulfonates (n: 2 FTS,n=4, 6 and 8), n:2FTOHs (n=6, 8 and 10), 2H,2Hperfuorodecanoic acid (8 : 2FTCA), PFOSA, 2H,2H,3H,3Hperfuoroundecanoic acid (8 : 3 FTCA),7H-perfuoroheptanoic acid (7HPFHpA), perfuoro-3,7-dimethyloctanoic acid (PF37DMOA) na PFBS, PFHxS, PFHpS, PFOS, PFDS, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoA, PFTrDA, PFTeDA na PFOS, PFOA, PFDoDA, PFHxS, PFNA, PFTeDA, PFTrDA, PFUnDA, PFBS, PFDA, PFHpA, PFHxA, PFBA, PFPeA, PFOSA 1763-23-1 (PFOS), 355-46-4 (PFHxS), 335-67-1 (PFOA), 375-95-1 (PFNA), 2058-94-8 (PFUnDA), 307-55-1 (PFDoDA), 72629-94-8 (PFTrDA), 376- 06-7 (PFTeDA), 375-73-5 (PFBS), 375- 22-4 (PFBA), 2706-90-3 (PFPeA), 307- 24-4 (PFHxA), 375-85-9 (PFHpA), 335- 76-2 (PFDA), 754-91-6 (PFOSA) PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFTrDA, PFTeDA, PFOS, PFOSA na total fluorine, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, EtFOSE, C3--C17 PFCAs, C4, C6, C8, C10 n:2 FTCA, C4, C6, C8, C10 n:2 FTUCAs, C3, C5, C7, C9 n:3 FTCA, C2-C10 PFSAs, fluorotelomer sulfonates (C4, 6, 8, 10 FTSAs), fluoroalkyl sulfonamido acetic acids (C4-C8 FASAA), N-methyl fluoroalkyl sulfonamide acetic acids (C4-C8 MeFASAA), ethyl fluoroalkyl sulfonamido acetic acids (C4-C8 EtFASAA), disubstituted perfluoroalkyl phosphinic acids (C4/C4-C8/C8 PFPIA), disubstituted polyfluorinated phosphate esters (C4/ C4-C10/C10 diPAP), fluorotelomer mercaptoalkyl phosphate esters (C6/C6-C10/C10 FTMAP), and ethyl perfluorooctanesulfonamido ethanol-based polyfluoroalkyl phosphate diester (C8/C8 SAmPAP) na 375-22-4 (PFBA), 29420- 49-3 (PFBS salt), 307-24-4 (PFHxA), 3871- 99-6 (PFHxS salt), 2043-47-2 (4:2 FTOH), 757124-72-4 (4:2 FTS), 335-67-1 (PFOA), 1763-23-1 (PFOS salt), 647-42-7 (6:2 TOF, targeted analysis of PFCAs (PFBA, PFHxA, FTOH), 29420-49-3 (6:2 FTS), 31506-32-8 PFOA, PFNA, PFDA), PFSAs (PFBS, PFHxS, PFOS), (MeFOSA), 4151-50-2 (EtFOSA), 2448-09- FTOHs (4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH), 7 (MeFOSE), 1691-99-2 (EtFOSE), 375-95- FTAs (6:2 FTA, 8:2 FTA, 10:2 FTA), FOSAs 1 (PFNA), 335-76-2 (PFDA), 678-39-7 (8:2 (MeFOSA, EtFOSA), FOSEs (MeFOSE, EtFOSE) FTOH) total fluorine na 21 volatile PFAS including 4:2, 6:2, 8:2, and 10:2 FTOH, N-MeFOSA, NEtFOSA, N-MeFOSE, and N- EtFOSE na E.g. PFBA, PFHxA, PFOA, PFNA, PFDA, PFUnDA, PFDoDa, PFGxS, PFOS, FOSA, PFPeA, PFHxA, PFTeDA, PFDS, PFHxS, L-PFOS na PFPA, PFHxA, PFHpA, PFOA, PFNa, PFDA, PFUnDA, PFDoDa, PFTrDA, PFTeDA, PFBS, PFHxS, PFHpS, PFOS and PFDS na PFBa, PFPeA, PFHxA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, (6:2, 8:2 an 10:2 FTOH), PFBS PFHxS, PFHpS, PFOS, PFDS, FOSA, N- MeFOSA, N-EtFOSA, N,MeFOSe, N-EtFOSE na PFOS, PFOA na 39 PFASs: PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFDS, PFOSA, MeFOSA, EtFOSA, MeFOSE, EtFOSE, PFPA, PFHxA, PFHpA, PF, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, 4:2 FTOH, 6:2 FTOH, 10:2 FTOH, 6:2 FTCA, 8:2 FTCA, 10:2 FTCA, 8:2 FTMAC, 10:2 FTMAC, 4:2 FTAC, 6:2 FTAC, 8:2 FTAC, 10:2 FTAC, 4:2 FTSA, 6:2 FTSA, 8:2 FTSA na PFOA na PFCAs (PFBA, PFHxA, PFHpA, PFOA, PFna, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA), PFASs (PFBS, PFHxS, PFOS), PAPs (6:2 diPAP, 6:2 monoPAP, 8:2 diPAP, 8:2 mono-PAP), FTOH (4:2, 6:2, 8:2), FTS (4:2, 6:2) 375-22-4 (PFBA), 307-24-4 (PFHxA), 37585-9 (PFHpA), 335-67-1 (PFOA), 375-95-1 (PFna), 335-76-2 (PFDA), 4234-23-5 (PFUnDA), 307-55-1 (PFDoDA), 72629-948 (PFTrDA), 376-06-7 (PFTeDA), 2942049-3 (PFBS salt), 3871-99-6 (PFHxS salt), 1763-23-1 (PFOS salt), 2043-47-2 (4:2 FTOH), 647-42-7 (6:2 FTOH), 678-39-7 (8:2 FTOH), 57677-95-9 (6:2 diPAP), 57678-01-0 (6:2 monoPAP), 678-41-1 (8:2 diPAP), 57678-03-2 (8:2 mono-PAP), 757124-72-4 (4:2 FTS), 29420-49-3 (6:2 FTS) APFO, PFOA, PFUdA, PFDoA, PFTrA, PFTeA na PFBA, PFPA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA, PFDoA, PFTrA, PFTeA, PFBS, PFHxS, PFHpS, PFOS, PFDS, 4:2 FTOH, 6:2 FTOH, 8:2 FTOH, 10:2 FTOH, PFOSA na 6:2 FTOH, 8:2 FTOH, 10:2 FTOH na C4-C14 PFCAs, C4, C6 ,C8 ,C10 PFSAs, 4:2, 6:2, 8:2 and 10:2 FTOHs, N-ethyl perfluorooctanesulfonamidoethanol (EtFOSE), N- Methyl perfluorooctane sulfona-midoethanol (MeFOSE), N-Ethyl perfluorooctane sulfonamide(EtFOSA) and N-Methyl perfluorooctane sulfonamide (MeFOSA) na 9 PFCAs (C4 to C12), 5 PFASs (C4, C6, C7, C8, C10) na (a) PFCAs (C4 - C14), PFSAs (C4, C6, C7, C8, C10) and FOSA-derivatives (FOSA, N-MeFOSA and N- EtFOSA), (n) FTOHs (6:2-, 8:2-, 10:2-FTOH) and FOSE-derivatives (N-MeFOSE and N-EtFOSE) na FTOH's. N, N-Me2FOSA, N-MeFOSA, N-EtFOSA, N- MeFOSA, N-ETFOSE na PFOS, PFOA na PFAS (i.e. C4-C14 PFCAs, C4,C6,C8,C10 PFSAs, 6:2 and 8:2 fluorotelomersulfonates (FTSs), PFOSA, 4:2, 6:2, 8:2, 10:2 FTOH na PFCAs, FTOHs na 1763-23-1 (PFOS) 754-91-6 (PFOSA) PFOS, PFOSA, N-Me-FOSA, N-Et-FOSA, N-Me-FOSE 24448-09-7 (N-Me-FOSE alcohol) alcohol, N-Et-FOSE alcohol, PFOS salt 1691-99-2 (N-Et-FOSE alcohol) TOP assay: PFPrA, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFBS, PFHxS, PFOS, PFDS, 6:2 FTS and 8:2 FTS na PFBA, PFPeA, PFHxA, PFOA, APFO, Na-PFOA, KPFO, Ag-PFO, F-PFO,PFNA, PFDA, PFUnA, PFDoA, PFTrA, PFTeA, PFBS,PFHxS, PFHpS, PFOS, PFOS-X, PFOSA, N-MeFOSA, N-EtFPSA, N-MeFOSE, 4:2-FTS, 6:2-FTS, 8:2-FTS; 10:2-FTS, N-EtFOSE, PFOSF, 4:2FTS, 6:2-FTS, 8:2-FTS, 10:2-FTS, PF-3,7-DMOA, PFDS, 7HPFHpA, 4HPFUnA 375-22-4, 2706-90-3, 307-24-4, 375-85-9, 335-67-1, 3825-26-1, 335-95-5, 2395-008, 335-93-3, 335-60-0, 375-95-1, 335-762, 2058-94-8, 307-55-1, 72629-94-8, 37606-7, 375-73-5, 355-46-4, 375-92-8, 1763-23-1, 2795-39-3, 29457-72-5, 29081-56-9, 70225-14-8, 56773-42-3, 754-91-6, 31506-32-8, 4151-50-2, 2444809-7, 2043-47-2, 647-42-7, 678-39-7, 865-86-1, 1691-99-2, 307-35-7, 7512472-4, 27619-97-2, 39108-34-4, 12022660-0, 251099-16-8, 172155-07-6, 335-773, 335-77-3, 1546-95-8, 34598-33-9 PFOA, its salts and PFOA-related compounds, namely Me-PFOA, Et-PFOA, 6:2 FTA, 8:2 FTA, 10:2 FTA, 6:2 FTMA, 8:2 FTMA 376-27-2 (Me-PFOA), 3108-24-5 (EtPFOA), 17527-29-6 (6:2 FTA), 27905-45-9 (8:2 FTA), 17741-60-5 (10:2 FTA), 2144- 53-8 (6:2 FTMA), 1996-88-9 (8:2 FTMA), 307-98-2 (7:1 FTA) Sampling sample amount used Nine oil-and-water repellent garments purchased from commercial vendors with fluorinated fabric coatings In addition, the durability of two fluorinated stain-resistant spray-on coatings, namely ScotchgardTM Fabric Crafts Protector and Forcefield Weathering: Threads Laundering: 5-10 x 30 mm 12 textiles marketed as stain-resistant bought in USA threads Four polyester samples. 30 mg in small pieces In addition to the three reference textiles, 7 medical textiles were obtained from Stockholm Healthcare (Region Stockholm). These included 1 surgical drape, 4 surgical gowns, and ambulance jacket all determined to contain an unknown fluoropolymer coating during 30 mg (2.7 cm2 ) 32 real textile samples of different fabrics (e.g., cotton, wool, and polyester) and 6 food packaging material samples (e.g., oil-proof hamburger wrapping paper) 1 x 1 cm2, 0.5 g 18 children's car seats 50-100 mg na 1.0 g 13 samples. textile samples originating from outdoor clothing (one pair ofoutdoor trousers, seven jackets, four fabrics for outdoor Circular pieces clothes,and one outdoor overal. All purchased with a diameter of 35.3 mm in Sweden (equals 9.79 cm2 real textile samples of different fabrics, as well as five popcorn bucket and six oil-proof hamburger wrapping paper samples, which were collected from local markets or purchased online na clothing fabrics 10 mg 30 samples of both used and unused fire fighting turnout gear from USA 250 mg 160 textiles purchased in USA. 2 x 2 cm waxed dental foss, textile, sewage sludge 15 real textile samples of different fabric na 94 consumer products that represent frequently used items on a college campus of Harvard University. These included: 45 food contact materials, 37 textiles, and 12 domestic products such as lens wipes, bandages, masks, and a shower curtain 1 0.03 g 2 textile samples were coated with 2 different DWR products 8 x 8 cm 300 products from 16 product lines placed on the market in four industrial sectors (Coated metal wares, textile products, leather products, household products) areas 100 cm2 cutted in 2 mm x 2 mm, for the liquid sample, 1 mL was collected The samples included fabrics pre-coated by a wet process (A1 and B1 from 3M) and by a plasma process (D1 and E1 from P2i), as well as coatings applied in the lab to white cotton (Testfabrics, West Pittston, PA, USA). 10 mm fiber 23 samples of building materials. 28 samples of industrial textiles. Mostly purchased directly but in some cases the manufacture's supplied the articles 1 gram 58 indoor dust samples and 73 urine samples from saleswomen 100 mg dust 0,5 ml urine Take a leather sample by mass using 1 g of 1,0 g 0,1 g of the leather leather. pieces leather samples 1 g large set of consumer products (food-contact papers, popcorn bag, outerwear textiles, childrens clothing, pillowcase, uhholstery cut from office chair) comprised of paper and textiles purchased by the Washington Department of Ecology in 2015 2 x 2 cm2 (0.3 +/- 0.01 g) In total 17 products were randomly selected from shelves in a number of Swedish retail stores and supermarkets for analysis (Cupcake forms, microwave popcorn bag, rinse aid, waterproofing shoe treatment, waterproofing textile treatment, shoe wax, floor polish, furniture polish, car wax). In total 29 samples of consumer products were collected in the previous study ( including food contact material, textiles, lubricants, car wax, table cloth, ski wax and more) Pressed pellets of 100-120 mg for TOF 350 consumer products purchased from 94 retail stores/vendors in April/May 2015 (paper and textile samples likely PFAS treated for water and oil repellency) 2 cm2 with 1 cm2 hole 7 papers consisted of all new materials purchased or acquired in 2017, including: white copier paper, five food-contact materials, and waterproof notebook paper, 9 textiles consisted of a plain white t-shirt, three office chair upholsteries from the years 1988a, 1988b, and 1993, respectively, an outdoor upholstery purchased in 2017, two articles of previously worn children's clothing (a swimsuit and outdoor vest), and an adult rain jacket purchased in 2015, as well as a piece of a used firefighter's jacket 1.5 x 1.5 cm Three jackets and three fabric from outdoor clothes from six different suppliers were purchased from Sweden Circular pieces with a diameter of 35,3 mm 126 samples in four categories: Textiles, Floor coverings, Electrical & Electronic equipment and plastics. All bought in Czech Republic 5 g 16 outdoor jackets were bought between August 2011 to March 2012 5 x 10 cm 32 textiles were purchased from stores in thailand: Diapers, shirts, pants, footwear, towels, uniforms, upholstry, carpetsl blankets, umbrellas, sunshades and tents Approx. 2 gram Twenty-two products were purchased and initially analysed for the content of total fluorine. Added to this were further eight samples from car seats, purchased as part of another study of chemicals in car seats, which was also carried out by DEPA. 10 cm2 Diluted PFOA textile samples was also used 5 cm x 5 cm In total 29 different samples were analysed. The sampling was concentrated on a few but wide variety of household products, such as cleaning products and polishes for indoor use and for cars and sprays to waterproof shoes or clothes, food contact paper and baking forms included some products less commonly analysed, such as ski wax, dental floss and tablecloths. The samples were purchased in the vicinity of Oslo in supermarket chains that are found all over Norway. depending on the article: 0.05 mL, 71.5-100 cm^2 or 0.020.16 g The test samples were three texiles spiked with pure chemials 0,5 g of textile (5 mm x 5 mm) 115 samples of consumer products including textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes. The individual samples analysed were bought from local retailers or collected by co-workers of the institute or local clubs (e.g. ski waxes from local skiing club). The sampled products span all quality levels from entry level to cutting edge products. The selection of the samples occurred randomly. na 54 consumer products from U.S. open market in the years of 2011 and 2013 (carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non-woven medical garments, floor waxes, food-contact paper, membranes for apparel, and threadsealant tapes) solid samples 0.05 g, liquid samples 100 L 45 furniture textile, carpet, clothing and food contactmaterial samples were purchased from three major retail stores inTroms and Trondheim during the period November2012eFebruary 201 10 x 10 cm 95 samples from 35 consumer products including carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non-woven medical garments, floor waxes, food-contact paper, membranes for apparel, and thread-sealant tapes. They were purchased from retail outlets in the United States between March 2007 and September 2011. 5 x 5 cm five impregnating agents and 16 outdoor jackets 2 squares 5 x 10 cm Air samples at 11 indoor sites taken in shops, offices, in a car, in a kitchen, workshops.They also tested liquid care products for textiles and 1 dm2 of textile for extraction shoes and emissions from surface-treated test textiles air emissions; 5-25 m3 of air not reported na 30 products in 6 different product groups: waterproofing agents, paint, coated fabrics, non-stick ware, electronics and fire fighting agents. They were purchased from retailers in Norway and Sweden. 1 g 13 items of outdoor clothing bearing well-known outdoor brand names na Solids (coated materials): at least 200 cm2 or 2 g, solids (non-coated): sampled according to EN ISO 8130-9 see sampling three reference textiles, seven medical textiles were obtained from Stockholm Healthcare (Region Stockholm). These included one surgical drape (6A), four surgical gowns (12, 17A, 21, and R10), and one ambulance jacket (35A), all determined to contain an unknown fluoropolymer coating during initial screening experiments, as well as a fluorine-free surgical TF - analysis: 0.3 - 0.8 mg drape (1A), which was used as a control. TOP assay: 3.5 - 14 mg according to EN ISO5089 Take a fabric test specimen in order to get at least 1 g of material and an area of at least 100 cm2. sampling is carried out according to EN ISO 5089 If the material is not suitable to provide area-based test specimens (fibres, yarns), take a test specimen by mass, using at least 1 g of material Pre- treatment Extraction weathering: Single threads from samples were exposed outdoor to wind, sun and rain for 12 weeks and were sampled at 4-week intervals Laundering: Small swatches were washed 9 times no extraction, pyrolysis single fibers were removed using gloves and tweezers no extraction, pyrolysis hydrolysis with 4% sodium hydroxide in water-methanol mixture (1:9) at 60 _x0003_C for 16 h Methanol cut using methanol-rinsed scissor, oxidation with Potassium persulfate and NaOH (TOP assay) SPE in methanol supramolecular solvent (SUPRAS)-based extraction, heptanol, tetrahydrofuran, and water mixed solvents Samples cut into small pieces and pre-cleaned with dichloromethane hexane/isopropanol followed by and methanol methanol/acetonetril homogenized sample, add standard for determining recovery rates ultrasonication in methanol, SPE Two pieces were cut out of each fabric. Oneof the pieces (9 cm12 cm) was exposed in an ATLAS weather-Ometer Ci 3000 to elevated UV radiation, humidity, and tempera-ture for 300 h (Table 2), which can be compared to the lifespan ofthe outdoor clothing Methanol dicationic ionic liquid (DIL) based easy ambient sonic-spray ionization (EASI), solvents (acetonitrile, methanol, acetone, isopropyl alcohol, dichloromethane, tetrahydrofuran, ethyl acetate, and na hexane) dillution ethyl acetate Cut into small pieces NaOH and methanol 5 squares from each sample were cut into pieces and pooled Methanol & ethyl acetate Derivatization was carried out by adding 50 l of 0.4 M DMF-DMA solution to 200 l PFCA solution or sample extract. Then the vials were closed and the sample was directly injected into GC-MS system All samples were weighed (100-500 mg) and shaken for 10 min after the addition of MTBE (2-5 mL). Subsequently, the samples were extracted for 30 min in an ultrasonic bath no pre-treatment no extraction cut using methanol-rinsed scissors, methanol extraction, XPS (not extracted mounted on carbon tape for XPS sample/ methanol extract) Fabrics were treated coated with DWR and washed several times No extraction na ultrasonically with methanol Samples were prepared by separating a thread from a swatch of fabric. The thread was then unwound with tweezers and a single fiber was removed. The fiber was placed on a glass slide and taped at both ends to pull the fiber taut. The fiber length was then measured with a stainless steel ruler and cut into 10 mm using an X-ACTO knife. no extraction, pyrolysis samples were cut and dried. liquid-solid extraction (LSE) or solid phase extraction (SPE). All solids were extracted via LSE. Coating 2 was available as an aqueous solution and directly enriched using SPE. LSE was performed with methanol (MeOH) and water. Dust: visible hair was removed. After Air drying it was stored at -20 until analysis Urine was stored at -20 until analysis ANC na Solvent Extraction (MeOH) Leather samples were cut as close ultrasound liquid extraction followed by to the scalp as possible SPE on Oasis Wax papers and textiles were cut from the original material using Sonification in ethyl acetate for FTOHs, methanol-rinsed scissors heated in methanol for PFASs sample was homogenized, shredded for TOF LC-MS: ultrasonic extraction with matrix dependent solvents (no further information), burning for TOF and absorbtion of combustion gases in buffer solution no no extraction papers and textiles were cut from the original material using methanol-rinsed scissors Sonification in methanol Prior to extraction dust particles were rinsedfrom the samples by adding 5 mL water to the pp tubes andtransferring the samples immediately into fresh 15 mL pp-tubes. Methanol Materials were crushed, chopped Methanol with the addition of ammonium or cut into small pieces acetate samples weighed and cut to small pieces. N-hexane Sampes cut into pieces and placed in desiccator Methanol Before extraction, the samples had 13C or deuterium-labelled ultrasonication in ethyl acetate (GC-MS), substances added. methanol (LC-MS/MS) textile cut into pieces na vortexing in methanol ultrasonification in methanol small samples ultrasound extraction with methanol differ depending on the respective matrix: ion pair extraction, acidic-alkaine sequential extraction or SPE with acetone, na hexane or methyl-t-butyl ether as solvent na Sonification in methanol Samples were extracted with methanol for ionic compounds and ethyl acetate for samples were cut into small pieces neutral PFASs two times for 15 min in an and spiked with masslabeled ultrasonic bath with vortex treatment in internal standard between solid products were cut into smaller subsections. Liquid products were subdivided into at least three 30-mL polypropylene vials solid and liquid sample extraction (Liu 2012, US EPA Report, EPA/600/R-12/585) The squares were weighed precisely and cut to small pieces. Each sample was spiked with a mixture of internal standards. (a) sonication in acetone/acetonitrile, (n) sonication MeOH textile samples were doped with the internal standards(13C-labelled Textile samples were extracted with hexane in ultrasonic bath supercritical fluid extraction (SFE), supercritical carbon dioxide (Sc-CO2) with na methanol Liquid and solid samples were homogenized methanol for ionic compounds and ethylacetate for FTOH na methanol for HPLC, MTBE for GC Sample materials need to ground as appropriate to ensure an efficient extraction process. Textile and paper shall be cut into pieces of maximum 1 cm2 before methanol is added. For grinding of polymers and granulates it is recommended to use EN ISO 6427 or ISO 9113. Sonification in methanol for textile, fabrics, leather and paper TF-analysis: In brief, textile samples (0.3-0.8 mg each, depending on the textile density) were cut using scissors (prerinsed with methanol and then dried) TOP assay: a 2.7 cm2 (30 mg) piece of reference textile or a 1.0 cm2 (3.5-14 mg, depending on the fabric density) piece of a medical textile was cut using scissors (prerinsed with methanol and then dried) TF-analysis: na TOP assay: after addidition of Milli-Q water (30mL). Potassium persulfate (0.48 g) and NaOH (0.456 mL of a 10 N solution) were then added, and the solution was vortexed and placed in the oven at 85 C for 6 h. Thereafter, the samples were allowed to cool and the pH was adjusted using concentrated HCl The test specimen shall be cut into extracted in an ultrasonic bath with pieces of 1 cm2 methanol The test specimen shall be cut into pieces of 1 cm2. The sampling preparation based on area is extracted in an ultrasonic bath with described in prEN 17681-1:2021. methanol Clean up Measurement no clean up no clean up no clean up GC-MS GC-PARCI-MS GC-MS extracts were concentrated UPLC-MS/MS, CIC diluted 1:1 (v/v) with methanol, filtered UHPSFC-(+)ESI-MS/MS Cleaned-up with Envi-Carb graphite by vortexing for 1 minY. Wu, G.Z. Miller, J. Gearhart et al.Environmental Pollution 268 (2021) 1154772 HPLC-MS, LC-MS and GC/MS (with/without TOP assay, UV treatment), PIGE na HPLC-MS / MS na LC-MS/MS na EASI-MS/MS na GC-MS na LC-MS/MS and particle induced gamma-ray emission (PIGE) The extract was divided into two equal aliquots of 5 mL each into new 15 mL PP tubes. One aliquot was subjected to solid phase extraction (SPE) for the analysis of PFAAs prior to oxidation, and the remaining 5-mL aliquot was subjected to chemical oxidation by the TOP assay HPLC-MS/MS no clean up na no clean up GC-MS dielectric barrier discharge ionization (DBDI) coupled with a benchtop ion trap mass spectrometer X-ray photoelectron spectrosopy (XPS), LC-(-)ESI-MS, LC-QTOFMS CIC filtration LC-MS/MS GC-PARCI-MS MeOH extracts were directly injected for FTOH determination or further enriched for nonvolatile PFASs. HPLC-MS/MS Dust was extracted three times. HPLC-MS/MS na LC-MS/MS This clean-up approach referred to the method by Olatz Zuloaga was published LC-MSMS Acquity UPLCTM BEH C18 (1.7m, 2.1100mm. The column temperature was set to 35 C. A gradient program was employed using 5 mM aqueous formic acid solution and methanol mobile phases. The flow rate of 0.08 mL/min and the volume injected was 5L. The gradient started at 35% methanol followed by an 8 min ramp to 87 % methanol. At 20 min, the ramp was decreased to 85 % methanol and at 25 min the ramp was decreased to 80 % methanol PIGE (total fluorine), GC-MS (FTOHs), HPLC-MS/MS (PFASs), TOP assay Targeted analysis with LC/MS-MS (Agilent HPLC 1290 Infinity LC-MS: (multi)-step-sample clean- Serie coupled with Agilent 6460A Triple Quad LC/MS-MSMS), up TOF by IC no Particle-Induced Gamma Ray Emission (PIGE) na GC-CSR-LVSI-MS, QTOF-MS (nontargeted analysis) no further cleaning. LC-MS/MS Following extraction, samples were cleanedup according to the procedures for PFAAs analysis described indetail elsewhere (Karaskova et al., 2016). GC-MS Following extractoin samples were washed with hexane HPLC-MS/MS na HPLC-MS/MS na GC-MS, LC-MS/MS, CIC na quenching effect on the fluorescence of quantum dots volume reduced to 2 mL, aliquot filtered UPLC-MS/MS for ionic PDAS and PAP, GC/MSD for FTOH na MS, HPLC-LTQ/Orbitrap differ depending on the respective matrix PFAA: HPLC-MS/MS FTOH: GC/CI-MS na GC/MS After centrifugation and solvent evaporation, an aliquot of1 mL extract was transferred for dispersive clean up with ENVI-Carb(50 mg, 1 mL, 100e400 mesh, Supelco, USA UPLC-MS/MS and GC-MS HPLC/MS/MS (a) evaporated, filtered, (n) SPE HPLC-MS/MS The presence of these precursors in samples, especially in extracts, could not be ruled out here, even though the applied cleaning procedure according to Szostek and Prickett (2004) seems to significantly reduce the FTOH precursor levels in samples GC-MS na HPLC/MS Centrifugation and solvent evaporation, clean up with ENVI- Carb and glacial acetic acid (for ionic PFAS) GC-MS na HPLC-MS/MS, GC-MS, SEM Concentrate the extract by a factor of 10 and use a clean-up if necessary. Active carbon clean-up and/or solid phase extraction (SPE) clean-up may be used. Transfer a known volume into a suitable LC sampling vial . If necessary dilute the original solution further and repeat the analysis LC-qMS, LC-tandemMS TF determination was carried out TF-analysis: na using an AQF-2100H combustion unit (Mitsubishi) that was TOP assay: solid phase extraction coupled to a Dionex ICS-2100 Integrion IC instrument (SPE). Oasis WAX (Thermo Scientific) SPE cartridges TOP assay: LC-MS/MS If the extract is turbid, centrifuge and decant the supernatant or filter it to a vial for LC/MS/MS analysis. LC-MS/MS Centrifuge the final extract of the test specimen and decant the supernatant to a vial for GC analysis. GC-MS/MS, GC-MS/PCI or GC-MS/EI Quantification method WAsorking range (ng/mL) Matrices na na internal standard method with 13C and/or 2H isotope-labeled 4:2, 6:2, 8:2 and 10:2 FTOHs Textiles textile textile Conversion between PFAS concentrations and fluorine equivalent concentrations na textiles internal standards 32 real textile samples of different fabrics (e.g., cotton, wool, and polyester) and 6 food packaging material samples (e.g., oil-proof hamburger wrapping paper) Internal standard foam and textiles internal standards, Calibration curves calibration 0.1 ng/ mL and 10.0 ng/mL textiles Internal standard na internal standardisation using mass-labeled internal standards na na Textiles real textile, popcorn bucket, and oilproof hamburger wrapping paper samples na Internal standard na Textiles internal standard internal standards na na Textiles textile, sewage sludge textiles paper and textile textiles mass labeled internal standard, calibration curve coated metal wares, textile calibration 5, 10, products, leather products, 25, and 50.0 mg/L and household products Internal standard textiles, paint, foan, glue, foil, na coatings An external calibration curve ranging from 0.1, 1, 5,10, 50 and 100 ng ml-1enabled us to discern the concentration ofeach extract. Prepare suitable calibration solutions using methanol, target compound solutions and the internal standard solution (suitable mass- labelled internal standards) na urine and dust Leather calibration curve e calibration curve in the range from 0.2 to 5 ng/mL leather internal standards papers (mainly food-contact material), textiles LC-MS: internal isotope-labeled standards (isotope dilution method) external inorganic fluorine standard (NaF) and external paper and textile standards with PFOA Consumer products, Textiles, FCM paper and textile internal standardisation using mass-labeled internal standards; FTOHs derivatives were quantified using the standard curve of 10:2 FTOH derivative Quantification was performed againstfive calibration solutions (0.1, 0.5, 2, 10,50 ng/mL) in methanol: water (1:1, v/v) prepared from a singlestock solution and the isotope-labeled ISs internal standards internal standards Internal standard (standard solutions) moisturizing creams (abbreviated CRE), founda_x0002_tions (FOUN), powders and eye shadows (POW), eye pencil (PEN) and shaving foams (SHAV) Textiles Textiles, matierials of wood and composite wood, plastics, foam, air conditioner components. electronic components Textiles Textiles linear regression through the execution of a series of calibration standards containing both labelled and unlabelled substances na textiles for children na 0.5 to 40mol L-1 extraction of textiles internal standardisation using mass-labeled internal standards na Consumer products, FCM internal standards extraction of textiles internal standardisation using mass-labeled internal standards internal standards textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non-woven medical garments, floor waxes, food-contact paper, membranes for apparel, and thread-sealant tape internal standards internal standardisation using mass-labeled standards Textiles, carpets and food contact materials carpet, commercial carpet-care liquids, household carpet/fabric-care liquids, treated apparel, treated home textiles, treated non-woven medical garments, floor waxes, food-contact paper, membranes for apparel, and thread-sealant tapes internal standards, Calibration curves na Outdoor jackets internal standard internal standard air samples, textiles solid matrices, paper, fabrics, sand internal standard food contact paper, textile, fire fighting foam, water proofing agents and lubricants, paint, leather, carpets, non-stick ware, printed circuit boards na na Outdoor jackets Quantify the samples by using the unextracted external calibration curve. When spiking with labelled reference solutions, the determination of the concentration is independent of possible errors made during injection. Also, errors caused by sample losses during distinct steps of sample pre-treatment or the adjustment of final sample extract volume as well as matrix effects in the sample are accounted for. Method is applicable for a concentration range for PFOS in Coated materials like paper, textile, the extract solution leather, carpets, clothes and of 0,5 g/l to 50 footwear, Non-coated materials, g/l. liquids The approach uses the total oxidizable precursor (TOP) assay for fingerprint-based structural elucidation and TF measurements (CIC) for quantification na 6 unknown side-chain fluorinated (SFP) coated medical textiles from Sweden Internal standard method range of 0,000 1 0,01 g/ml (0,001 - in textile materials (fibres, yarns, 1 g/ml for the fabrics) FTOH substances) and coated fabrics. The calibration is based on solutions containing the compounds of interest and internal standard solution of PFDodiAOMe The calibration curve for a substance is valid only for the measured concentration range. textile materials (fibres, yarns, fabrics) and coated fabrics Reported levels (ng/mL) info - validation of the method no levels were stated. They concluded that it was still possible to detect PFAS after weathering and laundering. na They were able to find fluorinated polymers in 10 out of 12 samples na FTOHs were found in much higher concentrations after hydrolyses compared to after normal extraction na Limitations ranged from 28 mg F/m2 (803 g F/g, textile 21) to 560 mg F/m2 (6560 g F/ g textile 35A) good agreement with reference values The inefficiency of the TOP assay on the oxidation of SFPs is also a notable area for improvement, but since we relied on TF measurements for quantification, this is not considered a limitation of the current methodology. Good linearity with correlation coefficients all PFDoA (19.85 g kg-1) greater than 0.99, six replicate measurements, and PFOA (12.49 g kg-1) relative errors less than 9% compared to HPLC- (textile sample) ESI-MS/MS Foam: ND-3,64 ng/g Fabric: ND - 93,4 ng/g Composite: ND-155 ng/g For the LC/MS and GC/MS analyses, a procedural blank and a matrix spike (spiking amount: 20 ng each of targeted PFAS) was processed along with every batch of 5e7 samples to evaluate the background contamination from laboratory operations Most of the PFAS show recovery rates between 80 na % to 100 % na The extraction and analysis Before weathering: method for the volatile PFASs was validated by Volatile PFASs: max. 350 assessment of the repeatability and the recovery. g/m2, ionic PFASs: max All textile samples of the repeatability and 45 g/m2 recovery assessment were extracted and analysed After weathering: in the same series. For both assessments the same Volatile PFASs: max. calibration curves were used. To assess the 7000 g/m2, ionic PFASs: repeatability of the method, two textile samples max 4500 g/m2 were extracted in triplicate on the same day. na ND, PFOA: 6.5 0.62 and calibration curves correlation coefficients 5.2 0.56 g/m2 of 0.9971 and 0.9993, triplicate analysis na na With PIGE (total fluorine measured): Used gear: up to 15.000 ppm Unused gear: up to 21500 ppm MS/MS: MDL - 850 ppb Calibration ranges are typically from 0.5 ng/g - 500 ng/g and process blanks were analyzed for each matrix, and 10 ng/g spike recovery measurement was performed for each analyte every eight samples. na sum of 13 PFAS: LOD 285 ng/g Quantification of PFAAs was based on an isotopic dilution method. Linear calibration (1/x weighted regression) curves were constructed for each analyte at 12 different concentrations (ranging from 0.02 to 200 ng/mL), and the calibration curves exhibited excellent correlation coefficients for all chemicals (r 2 > 0.999). A mid-point calibration standard and methanol were injected after every 10 samples to monitor for drift in instrumental sensitivity and carry-over of target chemicals between samples na 1,7-12 ng/g RSD: 1,9-6,2%, PFOA: 3200 nmol m-2 (0.38 mg kg-1) (carpet), PFBA: 960 nmol m-2 (0.60 mg kg-1) (disposable bowl), 45% F from a new upholstery sample Duplicate injection, precision experiments In addition, blanks and replicate-certified reference materials were 1330 g F/m2 for PA included during CIC measurements to ensure and 243 g F/m2 for PES/ absence of background contamination as well as CO fabrics accuracy and precision of the method. Of a total of 300 products, 51 were detected above the detection limits, which accounted for approximately 17% of the products tested. linearity of the calibration curve, instrument detection limit (IDL), method detection limit (MDL), and quality control. awning: 260 g/kg Seat Cover (car): 2-50 g/kg Coatings: 20-70 g/kg Foul (for facedes): 2-30 g/kg Blank samples were prepared with every extraction batch. Dust: 0 - 38,76 ng/g urine: 0 - 2000 ng/l na To eliminate the impact of background contamination, the instru-ments and apparatus that might possibly contain PFC sources, wesubstituted polyethylenefor all thefluoropolymer materials.One proce-dural blank was prepared after every ten samples. The mean value aver-aged over all the blanks was deducted from each result to correct forbackground levels The extent of matrix interferences varies considerably depending on the nature of the na samples, recoveries of all compounds spiked at 5 ng/L concentration level were in the range of 65-96%, na with a better RSD lower than 19% (n = 7). na Overall the levels of PFCAs in textiles were in the low g/m2 range and the level of 6:2 FTOH in the mg/m2 range 78-391 nmol F/cm2 (jacket), 129-597 nmol F/ cm2 (jacket high F), 161445 nmol F/cm2 (popcorn bag) and more replicate measurements on the same sample Total concentrations of ND-4000 ng/g (paper) and 67 to 180 000 ng/g (textile) continuing calibration verification (CCV) was analyzed at the beginning of each analysis no levels. Only recovery after different methods used The selected method was validated by a recovery assessment,by assessment of the repeatability, and the determination of thereproducibility Textiles: up to 77,6 g/kg Plastics: up to 0,384 g/kg OSB and wood: up to 18,3 g/kg (PFAS found The accuracy of method in 14 out of 14 samples) was evaluated using a set of spiked solidblank Car interior materials: up materials (polyurethane foam (n6) and sand to 3535 g/kg matrix blank(n10)) PFAS: 0,03-719 g/m2 PFOA: 0,02-171 g/m2 replicate measurements FTOH's 0,001-698 g/m2 on the same sample PFOS: 0,04 - 0,45 g/m2 PFOA: 0,42 - 10,97 g/m2 5 replicates of each sample The total concentration of the examined PFASs varied from 18 to 407 g/m. Total fluorine in products over detection limit 8,000 to 365,000 g/m Laboratory blanks consisting of reagents with the labelled standards added were extracted and analysed each time samples were analysed. In addition, the liquids used for migration and washing tests were also analysed to check for any blank values. In addition, recovery samples consisting of spiked textile, artificial saliva and laundry water were prepared. na Recovery of PFOA between 97 and 113% textile samples with PFOA was used to validate the reliability of the method. Recovery of PFOA between 97 and 113% Only PFOA, 8:2 FTOH and 6:2 FTOH were found in amounts at or above 1 g/m2 or 10 mg/ kg or mg/L na A validation was performed and several parameters such as linearity, matrix effect, LOQ, recovery and precision were studied PFOA: up to 2000 g/kg (ski waxes), up to 19 g/ m2 (outdoor textiles), up to 15 g/m2 (baking paper) PFBA: up to 200 g/kg (leather) PFBS: up to 120 g/kg (leather) accreditations according to DIN EN ISO/IEC 17025:2005, quality control standards 6:2 FTOH: ND - 331 g g(- 1), 8:2 FTOG: ND - 92 g g(-1), 10:2 FTOH: ND - 24 Internal audit pogram (IAP) standards analzed g g(-1) after each calibration, Daily quality check PFOA: up to 0,914 g/m2 Recoveries of internal Other PFCAs: up to standards, procedural and instrumental blanks and 1,022 g/m2 methoddetection limits are regularly monitored as FTOHs: up to 373 g/m2 quality criteria for theanalysis Individual PFCAs: ND2600 ng g-1 product In all analyzed jackets PFASs were determined in a range of 0.03 g/m2 to 719 g/m2 Recoveries not for all PFAS exaptable Problems mainly occurred for long-chained PFCAs (PFTrA and PFTeA) and PFDS, for which no isotopelabelled internal standard was available. Air samples: <0.04 ng/m3 all samples wereanalysed with to 285.8 ng/m3 , with 8:2 labelled FTOH standards enriched at the beginning FTOH being the ofthe analytical procedure and after doping N,N- dominant congener Me2FOSA into thefinalextract. extraction efficiencies (with double extractions) close to 100% for PFOA and 80% for na PFOS for both paper and fabric matrices As standard procedure, laboratory blanks, method detection limits (MDLs) and recoveries were examined. For each sample, a high resolution full scan spectra was used to control positive detections (typical mass tolerance 50 ppm). No laboratory contamination for any of the analyzed compound was detected Significant levels of PFOA (> 1 g/m2 ) 15) were found in six of 14 samples na na The recovery of labelled reference compound shall be in the range from 70 % to 125 % for the sample to be na considered valid. Four products contained C6-fluorotelomer-based SFPs (concentration range of 36-188 mg of C6F13/m2), one contained a C4sulfonamide-based SFP (718 mg of C4F9/m2), and one contained a C8fluorotelomer-based SFP (249 mg of C8F17/ m2) Laboratory background contamination was monitored by including procedural blanks (30 mL of MilliQ water; n = 3) with every TOP assay batch. A triplicate control of textile in milli-Q water without addition of oxidant was also performed with every TOP batch. Finally, to ensure the efficacy of the TOP assay when processing unknown textiles, samples of the nonfluorinated textile (1A) were spiked with 30 ng of individual PFAA precursors (6:2 and 8:2 fluorotelomer sulfonates; both n = 3) in methanol, dried, and then subjected to the TOP assay. TF measurements were analyzed together with a certified reference material (BCR-461, fluorine in clay), which showed good zgreement with reference values [average of n = 3 replicates = 552 7.3 (standard deviation) mg of F/kg vs a reference of 568 60 mg of F/kg] The inefficiency of the TOP assay for oxidizing SFPs is also a notable area for improvement (e.g., by modifying the concentration of persulfate) na na na na na na LoD (ng/mL) subgroup Measurement - generic name na GC-MS na GC-MS na GC-MS LC-MS/MS, CIC 0.2-1.6 g kg-1 (LOD), 0.6-3.2 g kg-1 (LOQ) LC-MS/MS na LC-MS/MS, GC-MS, TOP assay, PIGE na LC-MS/MS Limits of detection (LODs) of the ionic PFASs were between 0.02and 0.1mgm2, and LODs of the volatile PFAS were 0.3mgm2. PFOA: 0.5 (LOD), 0.8 (LOQ) g/m2, PFOS: 0.4 (LOD), 0.6 (LOQ) g/m2 LOD -3.5-19.4 pg of fluorine LC-MS/MS LC-MS/MS GC-MS MDL: 1,29-7,79 ng/ g LC-MS/MS LOD = 285 ng/g LC-MS/MS 0,2 ng/ml 5-10 g/kg GC-MS DBDI 1% for XPS, 0.0633.7 ng g-1 (MQL) for LC-MS/MS na XPS, LC-MS/MS, LCHRMS CIC MDLs between 0.47 and 1.42 mg/L LC-MS/MS GC-MS not in report LC-MS/MS LOD: 0,02 ng/ml 1,28 ng/ml quantification limit for PFOS of 0,2 mg/ kg is achieved LC-MS/MS LC-MS/MS 0.09-0.96 ng/L LC-MS/MS GC-MS: LOD = 0.37-2.4 g/m2, LOQ = 1.2-8.1 g/ m2; LC-MS: LOD = 0.016-0.18 g/m2, LOQ = 0.034-0.58 g/ m2 PIGE, GC-MS, LC-MS/ MS, TOP assay TOF: About 10 pellets must be processed to sustain a LOQ of 1 mg/kg fluorine (LOQ fluoride = 0.1 mg/l for IC) 13 nmol F/cm2 (papers), 24-45 nmol F/cm2 for textiles LC-MS/MS PIGE 30 and 77 ng/g (paper), 19 to 34 ng/g /(textile) GC-MS, LC-HRMS LOQs were reported (0.01-0.4mg/m2 LC-MS/MS na The limits of quantification ranged from 10 to 400 ng/m limits not mentioned GC-MS LC-MS/MS LC-MS/MS LOD = 20 mg/kg for total fluorine GC-MS, LC-MS/MS, CIC limit of detection 0.3mol L ? LOD = 0.030.15 g/m2, only qualitative for 6:2 monoPAP, 8:2 PAP, 6:2 diPAP, 8:2 diPAP LOQ between 2 and 20 mg/kg LC-MS/MS, GC-MS LC-HRMS LOQ (PFAA) = 0.1-0.5 g/kg or 0.02-0.5 g/ m2 LOD (FTOH) = 20000 g/kg quantification limit is the lowest calibration concentration LC-MS/MS, GC-MS GC-MS The MDLs for individual substances ranged from 0.005 to0.010mgm2and 0.5 to 2mgm2for ionic and neutral PFASsrespectively. LC--MS/MS na LC-MS/MS LOQ = 0.05 - 2 ng/ mL LC-MS/MS (LOQs) were 5 mg/ kg in most cases and 20 mg/kg in af few samples 0.71 ng mL-1 (PFOA), 0.12 ng mL-1 (PFOS); LOQ: 2.36 ng mL-1 (PFOA), 0.39 ng mL-1 (PFOS) GC-MS LC-MS/MS MDLs not reported na GC-MS LC-MS/MS, GC-MS, SEM na LC-MS/MS na na TOP assay, CIC 0.1 - 0.25 ng/mL (LOQ) except for the FTOH compounds a higher LOQ is obtained 20 ng/mL it is feasible to reach limits of detection (LoD) of 100 g/kg and limits of quantification (LoQ) of 250 g/kg LC-MS/MS GC-MS Title TOF-SIMS analysis of perfluoropolyether lubricant smear transferred from disk surface following laser heating TOF-SIMS ANALYSIS OF ACCUMULATED PFPE LUBRICANT SMEAR FOLLOWING LASER HEATING TOF-SIMS characterization of lubricants used in magnetic recording media A novel method for film thickness measurement of perfluoropolyether lubricant by secondary ion mass spectroscopy QUANTITATIVE SECONDARY ION MASS-SPECTROMETRY OF FLUOROCARBON POLYMERS Laser Desorption Ionization-Time-of-Flight Mass Analysis of Perfluoropolyether Monolayer Directly from Hard Disk Medium Surface Development of Extraction Methods for the Analysis of Perfluorinated Compounds in Leather with High Performance Liquid Chromatography Tandem Mass Spectrometry A pilot study of per- and polyfluoroalkyl substances in automotive lubricant oils from the United States Quantification of heavy perfluorinated organics by mass spectrometry Perfluoropolyether characterization by nuclear magnetic resonance spectroscopy and gel permeation chromatography Condition monitoring of perfluoropolyether (PFPE) lubricated components STUDY OF THE FORMATION AND BREAK OF LUBRICANT BRIDGE IN THE HEAD DISK INTERFACE USING MOLECULAR DYNAMIC METHOD Multianalyte profiling of per- and polyfluoroalkyl substances (PFASs) in liquid commercial products Authors Tani et al. Tani et al. Zhang et al. Zhu et al. Lorenz et al. Kudo et al. Zhang et al. Zhu et al. Saprygin et al. Karis et al. Silvestri et al. Journal year Microsystem Technologies-Micro-and Nanosystems-Information Storage and Processing Systems 2020 Vol. 26 Issue 1 Pages 79-88 Amer Soc Mechanical Engineers Applied Surface Science 2004 Vol. 231 Pages 336-341 2020 2018 2004 Applied Surface Science 2002 Vol. 189 Issue 12 Pages 53-58 Surface Science 1991 Vol. 250 Issue 1-3 Pages 112-122 Analytical Chemistry 2011 Vol. 83 Issue 14 Pages 5563-5569 2002 1991 2011 5th Annual International Conference on Material Science and Environmental Engineering, edited by K. Wang 2018 Environmental Technology & Innovation 2020 Vol. 19 Pages 8 Journal of Analytical Chemistry 2010 Vol. 65 Issue 14 Pages 1469-1474 Journal of Fluorine Chemistry 2002 Vol. 118 Issue 1-2 Pages 81-94 Society Machinery Failure Prevention Technology 1997 2020 2010 2002 1997 Dai et al. Amer Soc Mechanical Engineers 2016 Favreau et al. Chemosphere 2017 comments (t, nt, o) DOI link non-targeted na 10.1007/s00542-019-04447-7 https://doi.org/10.1115/ISPS-MIPE201 non-targeted 10.1016/j.apsusc.2004.03.085 non-targeted 10.1016/s0169-4332(01)01032-7 non-targeted non-targeted 10.1016/0039-6028(91)90714-4 10.1021/ac2005422 targeted 10.1088/1757-899x/301/1/012046 na 10.1016/j.eti.2020.100943 non-targeted 10.1134/s1061934810140054 non-targeted na 10.1016/s0022-1139(02)00197-5 no link na 10.1109/TMAG.2016.2626459 Also applied to AFFF 10.1016/j.chemosphere.2016.11.127 Name na na Films of lubricants, perfluoropolyether (PFPE) Fomblin Z-DOL, Z-TETRAOL, AM3001, and cyclo triphosphazene X-1P na na na perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnA), perfluorododecanoic acid (PFDoA), perfluorotridecanoic Acid (PFTrDA), perfluorotetradecanoic acid (PFTeDA) and perfluorooctanesulfonate (PFOS), perfluorooctane sulfonamide (PFOSA) C4-C12; perfluorobutanoic acid (PFBA), perfluoro-npentanoic acid (PFPeA), per_x0002_fluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), PFOA, perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnDA), and perfluorododecanoic acid (PFDoDA)] and four PFSAs [C4- C10; perfluorobutanesulfonate (PFBS), perfluorohexanesulfonate (PFHxS), PFOS, and perfluorodecanesulfonate (PFDS)] na na na na 41 targeted PFAs including PFCAs (C4-C16), PFSAs (C4, C6, C8, C10), ipPFNS, PFPAs (C6, C8, C10), FOSA, N-Me FOSA, NEt FOSA, FASAAs: FOSAA, N-MeFOSAA, N-EtFOSAA, NMeFOSE, N-EtFOSE, FTSAs (4:2, 6:2, 8:2 FTS), FTOHs (4:2, 6:2, 7:2s, 8:2, 10:2), 8:2 FTI, 8:2 FTAC, 8:2 FTMAC CAS (if available in source) na na na na na na na na na na na na na Sampling sample amount used perfluoropolyether (PFPE) lubricant D-4OH with a Demnum main chain and two hydroxyl functional units per end group na na magnetic recording media na direct na direct na PFPEs used were "Fomblin Z-Tetraol na leather samples 1 g automotive lubricant oils and hydraulic fluids 1g solutions on the basis of Freon_x0002_113, which contained PFC or PFPE in an amount ranging from 0.2 to 1000 g/mL na commercial PFPEs na direct na na na Household products included impregnation agents (n = 60), cleansers (n = 24), polishes (n = 18), lubricants (n = 7). A miscellaneous category of products (n = 23) was defined by various applications that included foamsuppressing agents for the chromium industry, paints, ski wax, 500 mg for LC-MS, 200 mg for inks and tanning substances. GC-MS Pre- treatment na na na Extraction na na na na na na na NaTFA solution (0.2 mg/mL in THF/HFIP = 1:1) was sprayed on the disk surface na ultrasound liquid extraction followed by SPE on Oasis Wax na na na na na na na na na na na LC-MS: dissolved in 10 mL water, adding methanol/water, ammonium acetate (pH 4), GC-MS: dissolved in 10 mL methanol, filtration LC-MS: SPE with methanol/ ammonium acetate (50:50) Clean up Measurement na time-of-flight secondary ion mass spectrometry na na TOF-SIMS na TOF-SIMS na Secondary ion mass spectrometry (SIMS) i na LDI-TOF-MS LC-MSMS Acquity UPLCTM BEH C18 (1.7m, 2.1100mm. The column temperature was set to 35 C. A gradient program was employed using 5 mM aqueous formic acid solution and methanol mobile phases. The flow rate of 0.08 mL/min and the volume injected was 5L. The gradient started at 35% methanol followed by an 8 min ramp to 87 % methanol. At 20 min, the ramp was decreased to 85 % na methanol and at 25 min the ramp was decreased to 80 % methanol LC-MS/MS Betasil C18 100 mm 2.1 mm, 5.0 m column. The mobile phase consisted of methanol (A) and 20 mM ammonium acetate in water (B). The optimized mobile phase gradient flow was as follows: 10% A from 0.0 to 0.1 min, 10% to 30% A from 0.1 to 1.0 min, 30% to 99% A from 1.0 to 8.0 min, 99% A from 8.0 to 12.0 min, 99% to 10% A from 12.0 to 12.5 min, and 10% A from 12.5 to 17.5 min, which was set at a flow rate of 0.3 mL/min. na total oxidizable precursor (TOP) assay a gas chromatograph or by means of direct probe under particular na temperature conditions nuclear magnetic resonance (NMR) spectroscopy and gel permeation na chromatography (GPC) na na na na LC-MS: adding ammonium hydroxide in methanol (0.5 %), neutralized with acetic acid LC- MS/MS, GC-MS/MS for FTOHs, FTI, FTAC, FTMAC Quantification method Working range (ng/mL) As qualitative na na monitor the thickness and molecular weights of the lubricant na thickness is determined by etching time for the lubricant backbone fragments CF2O and C2F4O to converge or by monitoring the maximum position of the deth profile of CH fragment na na na qualitative na Matrices na na lubricant lubricant polyperfhtoroet her films o disk surface na na leather na na na na characterize, chain composition end groups, and molecular weight distribution na na na lubricants lubricant lubricant na na na internal standardisation using mass- labeled standards na na household products (impregnation agents, cleanser, polishes), lubricants, foamsuppressin g agents for the chromium industry, paints, ski waxes, inks, tanning substances, reported levels (ng/mL) na na na 11-79 A 6-160 A na info - validation of the method na na na good linearity na na Limitations na na na na na na recoveries of all compounds spiked at 5 ng/L concentration level were in the range of 65-96%, na with a better RSD lower than 19% (n = 7). na Following oxidation, lubricant extracts excellent regression coefficients for all chemicals yielded PFAA concen_x0002_trations (r2 > 0.999). Six procedural blanks, three for un- up to two orders of magnitude higher oxidized extracts and three for oxidized extracts, (range: 196-8300 ng/g; mean: 1840 were analyzed with the real samples. ng/g) recoveries of PFAAs were 84.9%-121% and than those measured prior to 77.1%-119% for non-oxidative and oxidative oxidation (5.96-344 ng/g; 71.6 ng/g) methods na na na na na na na na na na na na na 55% of all samples contained at least one PFAS between 0.1 and 25'000 mg/kg of product, with the majority of products falling within the 100e1000 mg/kg range na na LoD (ng/mL) na na na subgroup Measurement - generic name na LC-HRMS na na TOF-SIMS na na TOF-SIMS na na TOF-SIMS na na 0.09-0.96 ng/L na LC-MS/MS 0.010 to 0.160 ng/g na 0.1 g/mL na na na na LC-MS/MS GC-MS NMR, GPC na na LOQ: 0.5-2 ng/mL (LCMS), 2-10 ng/mL (GC-MS) na LC-MS/MS, GCMS Title Authors Concentrations of organic contaminants in industrial and municipal bioresources recycled in agriculture in the UK. Rigby et al. 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A validated analytical method for the determination of perfluorinated compounds in surface-, sea- and sewagewater using liquid chromatography coupled to time-of-flight mass spectrometry Wille et al. DIN 38407-42:2011 - Standard methods for the examination of water, waste water and sludge na DIN 38414-14 - German standard methods for the examination of water, waste water and sludge - Sludge and sediments (group S) - Part 14: Determination of selected polyfluorinated compounds (PFC) in sludge, compost and soil - Method using high performance liquid chromatography and mass spectrometric detection (HPLC-MS/MS) (S 14) na Per- and Polyfluoroalkyl Substances in Landfill Leachate: Patterns, Time Trends, and Sources Benskin et al. 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Investigation of waste incineration of fluorotelomerbased polymers as a potential source of PFOA in the environment Taylor et al. Silicon photovoltaic modules at end-of-life: Removal of polymeric layers and separation of materials. Fiandra et al. Perfluorochemicals in wastewater treatment plants and sediments in Hong Kong Ma et al. Wide-scope target analysis of emerging contaminants in landfill leachates and risk assessment using Risk Quotient methodology Nika et al. Contaminants in landfill soils - Reliability of prefeasibility studies Hlzle Polyfluoroalkyl compounds in landfill leachates Busch et al. Focused ultrasound solid-liquid extraction of perfluorinated compounds from sewage sludge Martnez-Moral et al. Spatial distribution and importance of potential perfluoroalkyl acid precursors in urban rivers and sewage treatment plant effluent - Case study of Tama River, Japan Ye et al. 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Zhou et al. Multi-residue method for the determination of over 400 priority and emerging pollutants in water and wastewater by solid-phase extraction and liquid chromatography-time-of-flight mass spectrometry Robles-Molina et al. Trace determination of perfluorooctane sulfonate and perfluorooctanoic acid in environmental samples (surface water, wastewater, biota, sediments, and sewage sludge) using liquid chromatography - Orbitrap mass spectrometry Zacs et al. HPLC-MS/MS methods for the determination of 52 perfluoroalkyl and polyfluoroalkyl substances in aqueous samples Gremmel et al. Identification and Fate of Aqueous Film Forming Foam Derived Per_x0002_and Polyfluoroalkyl Substances in a Wastewater Treatment Plant Houtz et al. Journal Year Comments The Science of the total environment (i) land applied materials: treated sewage sludge (biosolids), meat and bone meal ash (MBMA), poultry litter ash (PLA), paper sludge ash (PSA) and compost-like-output (CLO), and (ii) bedding materials: recycled waste wood (RWW), dried paper sludge (DPS), paper sludge 2021 ash (PSA) and shredded cardboard Environmental Science & Technology 2012 33 urban runoff samples Chemosphere. 2016 Sep;159:638-646 6 sewage treatment works (STW) effluent discharges as well as concentrations in 5 rain2016 driven street runoffs and field drainages Environ Sci Technol. 2017 Feb 21;51(4):2197-2205 70 PFASs in 95 samples of leachate were 2017 measured in a survey of U.S. landfills Environmental Pollution Volume 159, Issue 1, January 2011, Pages 125-132 2011 air samples Environmental Science & Technology, 19 Jan 2018, 52(3):1301-1310 air, dry deposition, and plant leaves at two 2018 different landfills The Science of the total environment 2019 ambient air and leachate J Hazard Mater. 2013 May 15; 0: 413-418 2013 biosolids Journal of Environmental Management 165 (2016) 88e95 Waste Manag Environ Int biosolids from a municipal water resource 2016 recovery facility (WRRF) determine the gas composition, attenuation, and emission of fluorocarbons in a monofill shredder residue landfill cell by field 2010 investigation digested sewage sludge 2013 long-chain perfluorinated acids Chemosphere 2015 digested sewage sludges Environmental Science & Technology 2013 effluent and influent Water Res Environ Sci Technol. 2015 Oct 20;49(20):12333-41 Emerging contaminants Pharmaceuticals Pesticides Carbamazepine 2015 Wastewater reuse 2015 Extended Suspect and Non-Target Environmental pollution (Barking, Essex : 1987) 2019 groundwater surrounding legacy landfills Environmental pollution (Barking, Essex : 1987) indoor dust samples collected from urban, 2020 industrial, and e-waste dismantling areas Environmental science and pollution research international industry effluent 2013 landfill leachate and sludge Journal of environmental sciences (China) 2017 influent and effluent sewage water and sludge Environ Sci Pollut Res Int. 2012 Jun;19(5):1405-15 2012 influents and effluents and sludge samples J Chromatogr A J Chromatogr A landfill 2014 (Leachates coming from landfills) 2012 landfill leachate The Science of the total environment 2019 landfill leachate Journal of hazardous materials 2016 landfill leachate and biosolids Chemosphere 2011 landfill leachates Chemosphere 2021 landfills Environmental science. Processes &amp; impacts landfills (leachate and sediment from ten Norwegian 2019 landfills) Chemosphere Chemosphere 2021 leachate from a Waste-to-Energy stockpile leachate samples analyzed and gemfibrozil was detected in samples from four of the five2015 landfill sites. The Science of the total environment leachate, fly ash and bottom ash produced from three MSW incineration plants in 2021 southern China. Environmental pollution (Barking, Essex : 1987) 2021 leachate-impacted groundwater Waste Management Volume 107, 15 April 2020, Pages 191-200 leachates from municipal solid waste (MSW), construction and demolition (C&amp;D), MSW ash (MSWA), and a mixture of MSWA and MSW 2020 with landfill gas condensate (MSWA/MSW-GC) 2021 Management of Waste, no analytical method Environ Sci Technol. 2015 Jun 2;49(11):6519-27 2015 municipal sewage sludge samples Journal of Chromatography A Volume 1217, Issue 43, 22 October 2010, Pages 6616-6622 2010 na 2011 na 2011 na Environ Sci Technol. 2012 Nov 6;46(21):11532-40 2012 na Analytica Chimica Acta Volume 881, 30 June 2015, Pages 98-106 2015 na J Chromatogr A. 2015 Sep 25;1413:107-16 2015 na Sci Total Environ. 2015 Aug 15;524525:23-31 2015 na Chemosphere, Volume 168, February 2017, Pages 399-407 2017 na Journal of Hazardous Materials Volume 331, 5 June 2017, Pages 132141 2017 na Environmental Science & Technology 2018 na Environ. Sci. Technol. 2019, 53, 11093-11101 2019 na Environmental Science and Technology Letters 6(6): 372-377. 2019 na Science of The Total Environment Volume 695, 10 December 2019, 133810 2019 na J Anal Methods Chem. 2021 Apr 21;2021:5564994 2021 na 2015 (2020 revised) na Environ. Sci.: Processes Impacts, 2021,23, 588 2021 na Sci Rep Croat. Chem. Acta 84 (3) (2011) 439- 446. Nafion N117 membrane thermolysis products in water and methanol Additionally, this study provides an analytical justification of the LC/ESI-MS/MS method for characterizing the degradation products of 2015 polymer electrolyte membranes New methods developed for the determination using the HPLC with fluorescence detection and capillary electrophoretic methods are discussed, as well as the new method for the 2011 determination of total organic fluorine (TOF). Journal of chromatography. A new validated protocol 2011 sewage sludge Chemosphere. 2014 Sep;110:17-22 2014 no focus on PFAS analysis but on combustion Waste Manag preliminary mechanical treatment to remove fluorinated polymers determining the quantity and quality of the recovered materials The gaseous products of the polymeric degradation have been characterized by gas chromatography-mass spectrometry (GC-MS) 2019 analysis. Environmental pollution (Barking, Essex : 1987) quantification of PFCs in environmental samples without having to make internal modifications to a liquid chromatography 2010 system J Hazard Mater Waste Manag 2020 Raw and treated leachate reliability of prediction of the two investigation methods 2017 fluorine (leachate) Environmental pollution (Barking, Essex : 1987) 2010 samples of untreated and treated leachate Talanta 2013 sewage sludge Water Res. 2014 Dec 15;67:77-85 2014 sewage treatment plant (STP) effluents Chemosphere 2020 sludge Chemosphere Volume 92, Issue 3, July 2013, Pages 329-335 Analytical chemistry 2013 sludge from wastewater treatment plants software application 2020 landfill leachate as well as in leachate foam The Science of the total environment 2021 soil adjacent to a landfill Environmental Science & Technology, 15 Oct 2010, 44(22):8390-8396 Environmental Science & Technology 2020 Vol. 54 Issue 14 Pages 86408648 2010 soil samples from sludge 2020 targeted Environ Sci Technol 2021 Vol. 55 Issue 4 Pages 2346-2356 Waste Manag Water Res. 2015 Apr 1;72:28-39 Waste Manag. 2010 Nov;30(11):2153-62 Chemosphere 2021 targeted and untargeted The elemental compositions of the PV sample and the residue condensed organic products have been determined. The gaseous degradation products have been characterized 2019 bThyigsapsilcohtrsotmudaytosghroawpehdictahneaolycscisur(rGeCn)c.e of organic contaminants including pharmaceuticals and personal care products (PPCPs), perfluoroalkyl surfactants (PFASs), polybrominated diphenyl ethers (PBDEs), and polychlorinated biphenyls (PCBs) in septic effluents, adjacent lake water samples, household drinking water in homes that use lake water or a well adjacent to the lake as a 2015 source of drinking water Waste from the open SR landfill cell at the AV Milj landfill in Denmark was sampled at three 2010 locations. waste gas ideal method to pre-screen the presence of PFCs before a non-distinguishable TNMOC analyzer is applied to approximate the VOC level as part of the integrated effort to monitor 2020 VOC in flue gas Chemosphere 164 (2016) 322e329 2016 wastes Journal of chromatography. A 2018 wastewater Analytical and Bioanalytical Chemistry 2019 wastewater J Chromatogr A wastewater 2021 (developed for application to wastewater) Anal Bioanal Chem wastewater 2014 (effluent wastewater) Journal of hazardous materials wastewater (liquid and solid samples from five different 2014 wastewater treatment types) Water research wastewater (municipal wastewater samples) 2016 Effluent samples Environ Sci Technol. 2017 Aug 15;51(16):8953-8961 wastewater (Municipal Wastewater Treatment Plants) 2017 influent, secondary effluent, and sludge Environ Sci Technol 2021 wastewater (WWTP) Environmental monitoring and assessment 2015 wastewater and sludge J Chromatogr A. 2019 Sep 13;1601:79-85 2019 wastewater samples Sci Total Environ water- and particle phase of landfill leachates 2010 perfluorinated compounds (PFCs) Environmental monitoring and assessment water near waste recycling municipal dumping site 2013 e-waste recycling site Chemosphere WWTP (Biosolids samples were collected from 19 2021 Australian WWTPs ) Arch Environ Contam Toxicol. 2019 Feb;76(2):206-215 WWTP (effluent from a wastewater treatment plant ) 2019 wastewater from firefighter training area Chemosphere. 2018 Oct;208:975-983 WWTP (influent, effluent and biosolids samples from 2018 14 WWTPs ) Environmental Pollution WWTP 2014 (wastewater treatment plant effluent) Chemosphere 2015 WWTP influent, effluent and sludge Heliyon WWTP solid and aqueous samples. 2019 Method development Talanta WWTP (8 influents and 11 effluents of wastewater 2018 treatment plants) J Hazard Mater WWTP (biosolids samples from twenty pan-Canadian 2020 wastewater treatment plants (WWTPs)) Environmental Science & Technology, 14 Jan 2014, 48(3):1811-1818 WWTP (detected peaks from 10 Swiss wastewater treatment plant samples) 2014 included non targeted and suspect screening Science of the Total Environment 631-632 (2018) 660-667 WWTP (effluent from Bugolobi wastewater treatment 2018 plant) Environmental science and pollution research international WWTP (In a previous study, the concentrations of PFOA and PFOS in grab samples collected from the waste water treatment plant (WWTP) of 2010 Bayreuth) Journal of Chromatography A, 1515 (2017) 45-53 WWTP (influent and effluent of a wastewater 2017 treatment plant) Environment international WWTP (influent, effluent, and excess sludge from six 2019 WWTPs) J Chromatogr A. 2014 Jul 11;1350:3043 2014 J Chromatogr A . 2016 Nov 18;1473:109-121 2016 Analytical and Bioanalytical Chemistry 2017 Chemosphere. 2018 Oct;208:975-983 2018 DOI link PFAS 10.1016/j.scitotenv.2020.142787 10.1021/es302274g PFOA (335-61-1), PFDA (335-76-2), PFDoDA (307-55-1), PFHxS (355-46-4), PFOSA (754-91-6), PFNA (375-95-1), PFUnDa (2056-94-8), PFBS (375-73-5), PFOS (1763-23-1) PFPeA PFDA PFUnA PFDoA PFBS PFHxS PFDS FOSA N-EtFOSAA N-MeFOSAA 8:2 FtS PFAS PFTrA PFTeA N-EtFOSE 10.1016/j.chemosphere.2016.06.039 PFBS, PFNA. PFOA, PFOS 10.1021/acs.est.6b05005 PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, 6:2 FTCA, 8:2 FTCA, 3:3 FTCA , 5:3 FTCA, 7:3 FTCA, PFBS, PFPS , PFHxS, PFOS, 6:2 FTSA, 8:2 FTSA , MeFBSAA , MeFPeSAA , MeFHxSAA , MeFHpSAA , MeFOSAA, EtFBSAA , EtFPeSA , EtFHxSAAe , EtFOSAA; 10:2 FTCA, 6:2 FTUCA, 8:2 FTUCA, 9:3 FTCA , PFHpS , 4:2 FTSA , FBSAA , FPeSAA , FHxSAA , FHpSAA , EtFHpSAA; PFUnDA, PFDoDA, PFTriDA, PFTeDA , PFPeDA , PFHxDA , PFHpDA , PFOcDA , 4:2 FTCA , 4:2 FTUCA , 10:2 FTUCA , PFNS , PFDS, FOSAA , 4:4 PFPIA , 4:6 PFPIA , 6:6 PFPIA, 6:8 PFPIA, 8:8 PFPIA, 4:4 diPAP , 4:6 diPAP , 6:6 diPAP, 6:8 diPAP , 8:8 diPAP, 8:10 diPAP , 10:10 diPAP , 6:2 FTMAP , 6:2/8:2 FTMAP , 8:2 FTMAP , 8:2/10:2 FTMAP , 10:2 FTMAP , 8:8 SAmPAP 10.1016/j.envpol.2010.09.023 na 10.1021/acs.est.7b05385 10.1016/j.scitotenv.2019.135832 10.1016/j.jhazmat.2013.03.016 6:2, 8:2, and 10:2 FTOHs; N-methyl and N-ethyl (N-Me/Et) FOSAs; N-methyl and N-ethyl (N-Me/Et) FOSEs, 6:2 and 8:2 diPAPs; TFA, PFPrA, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, and PFDoDA); C4, C6, and C8 perfluoroalkane_x0002_sulfonic acid (PFSA) analogue TOP (total oxidazable precursors) C2-C3 PFAA-precursors Perfluorobutanoate (PFBA) Perfluoropentanoate (PFPeA) Perfluorohexanoate (PFHxA) Perfluoroheptanoate (PFHpA) Perfluorooctanoate (PFOA) Perfluorononanoate (PFNA) Perfluorodecanoate (PFDA) Perfluoroundecanoate (PFUnDA) Perfluorododecanoate (PFDoDA) Perfluorobutane sulfonate (PFBS) Perfluorohexane sulfonate (PFHxS) Perfluorooctane sulfonate (PFOS) Perfluorooctane sulfonamide (PFOSA) 10.1016/j.jenvman.2015.09.023 10.1016/j.wasman.2010.03.033 10.1016/j.envint.2013.08.020 perfluorobutanoic acid (PFBA), perfluropentanoic acid (PFPeA), pefluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), PFOA, perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), per- fluoroundecanoic acid (PFUnA), perfluorobutanesulfonic acid (PFBS), perfluorohexanesulfonic acid (PFHxS), PFOS, and per- fluorodecanesulfonic acid (PFDS) CFC-11, CFC-12, HFC-134a, HCFC-141b, HFC245fa, HCFC-21, HCFC-22, HCFC-31, HFC-32, and HFC-41 na 10.1016/j.chemosphere.2014.07.045 perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), perfluorooctanoic acid (PFOA), perfluorononaoic acid (PFNA), perfluorodecanoic acid (PFDA), sodium perfluorobutane sulfonate (PFBS), sodium perfluorohexane sulfonate (PFHxS), sodium perfluorooctane sulfonate (PFOS) 10.1021/es401525n chlorinated polyfluorinated ether sulfonate (locally called F-53B, C8ClF16O4SK), PFOS 10.1016/j.watres.2014.11.034 10.1021/acs.est.5b03454 10.1016/j.envpol.2019.02.018 10.1016/j.envpol.2020.114461 PFOA Perfluorheptanoic acid Perfluorooctanoic acid Perfluorononanoic acid 17 PFAS: PFBA; PFPeA;FFHxA; PFHpA; PFOA; PFNA; PFDA ; PFUnDA; PFDoDA; PFBS; PFPeS; PFHxS; PFHpS; PFOS; PFDS; 6:2 FTS; 8:2 FTS 25 PFAS: PFBA, PFPeA. PFHxA, PFHpA, PFOA, PFNA, PFDA, PFunDA, PFDoDA, PFBS, PFOS, 6:2 FTUCA, 8:2 FTUCA, 6:2 Cl-PFESA, 8:2 Cl_PFESA 10.1007/s11356-013-1518-z PFHxA, PFOA, PFOS, PFDA 10.1016/j.jes.2017.05.004 PFCA, PFSA, FTSA, FTCA, FTUCA: PAP, PFPA, PFPiA 10.1007/s11356-011-0727-6 PFDoA PFUnA PFDA PFNA PFOA PFHpA PFHxA PFPeA PFBA PFOS PFHxS 10.1016/j.chroma.2014.07.056 10.1016/j.chroma.2012.05.077 70 different PFASs (PFPA), perfluorohexanoate (PFHxA) perfluoroheptanoate (PFHpA), perfluoronanoate (PFNA), perfluorodecanoate (PFDA), perfluoroundecanoate (PFUnA), perfluorododecanoate (PFDoA), perfluorotetradecanoate (PFTA) and perfluorobutanesulfonate (PFBS) 10.1016/j.scitotenv.2019.02.203 16 PFAA 10.1016/j.jhazmat.2016.03.031 PFOA , PFOS , PFHxA , PFNA , PFDA , PFBS , PFUnDA , PFDoDA , PFTrDA , PFTeDA 10.1016/j.chemosphere.2010.11.072 PFBA PFPA PFHxA PFOA PFNA PFDA PFUnDA PFDoDA PETrDA PFTDA FPUEA PFBS PFHxS PFOS PFDS FtS MEFBSA MeFBSAA FOSA FOSAA ME-FODAA Et-FOSAA 10.1016/j.chemosphere.2021.130167 10.1039/C9EM00170K PFPeA, PFHxA, PFHpA, PFOA, PFNa, PFDA, PFUDA, PFDoDA, PFTrDA, PFTeDA, PFHxDA, PFBS, PFHxS, PFOS, PFDS 28 PFASs short-chain PFCAs(PFBA, PFPeA and PFHxA), a short-chain PFSA (PFBS), long-chain PFCAs (PFHpA, HPFHpA, PFOA, PFNA, PFDA, PF3,7-DMOA, PFUnDA, PFDoA, PFTrA, PFTA and PFHxDA), long-chain PFSAs (PFHxS, PFHpS, PFOS and PFDS), as well asuo-rotelomer sulfonates (FTSAs: 4 : 2 FTSA, 6 : 2 FTSA and 8 : 2FTSA), auorotelomer alcohol (FTOH: 8 : 2 FTOH) and PFOS-precursors (peruorosulfonamides (FOSAs): FOSA, EtFOSA,MeFOSA and peruoroalkylsulfonamide alcohols (FOSEs):EtFOSE and MeFOSE 10.1016/j.chemosphere.2021.130380 34 PFAS- E.g. PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, 4:2 FTSA, 6:2 FTSA, 8:2 FTSA Also EOF (Extractable organofluorine) were measured 10.1016/j.chemosphere.2015.02.030 PFOA PFOS 10.1016/j.scitotenv.2021.148468 (PFBA), (PFPeA), (PFHxA), (PFHpA), (PFOA), (PFNA), (PFDA), (PFUdA), (PFDoA), (PFTrDA), (PFTeDA), (PFBS), (PFHxS), (PFHpS), (PFOS), (PFDS), (PFHxPA), (PFOPA), (PFDPA), (6:2 diPAP), (8:2 diPAP), M2PFOA), (M4PFOS)). M2PFOA 10.1016/j.envpol.2021.116474 PFBA, PFOA, PFDoDA, PFBS, PFDS, PFPeA, PFNA, PFTriDA, PFHxS, PFECHS, PFHxA, PFDA, PFTeDA, PFOS, FOSA, PFHpA, PFUnA 10.1016/j.wasman.2020.03.034 7 carboxylic acids, 3 sulfonic acids, and 5:3 fluorotelomer carboxylic acid PFOS PFOA 10.1021/acs.est.5b01010 Cl-PFAESs, F-PFAESs, PFSAs, FTSAs 10.1016/j.chroma.2010.03.054 PFBS PFHxS PFOS PFDS PFPAa PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTeA PFOSA PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFBS PFHxS PFOS C4-C10 PFCA C4-C8 PFSA 10.1021/es302471n PFBS, PFHxS, PFOS, PFDS, PFBA, PFPeA, PFHxA, PFHpA, PFOS, PFNA, PFDA; PFUnDA, PFDoDA, PFTDA, FOSA, FOSAA, MeFOSAA, EtFOSAA, 6:2 FTCA, 8:2 FTCA, 10:2 FCTA, 6:2 FTUCA, 8:2 FTUCA, 10:2 FTUCA 10.1016/j.aca.2015.04.015 PFHxA, PFHpA, PFOA, PFNA. PFDA, PFOS 10.1016/j.chroma.2015.08.016 4:2 FTOH, 6:2 FTOH, 8:2 FTOH and 10:2 FTOH, NMeFOSA, N-EtFOSA, N-MeFOSE and N-EtFOSE 10.1016/j.scitotenv.2015.03.111 pentafluoropropionic acid (PFPrA), perfluorobutyric acid (PFBA), perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnA), perfluorododecanoic acid (PFDoA), perfluorotetradecanoic acid (PFTA), perfluoro-1butanesulfonic acid potassium salt (PFBS), perfluorohexanesulfonic acid potassium salt (PFHxS) and perfluorooctanesulfonic acid (PFOS) 10.1016/j.chemosphere.2016.10.072 PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTeDA, PFBS, PFHxS, PFOS 10.1016/j.jhazmat.2017.02.006 PFOA, PFOS, perfluorohexanoate (PFHxA), perfluoroheptanoate (PFHpA), perfluorononanoate (PFNA), perfluorodecanoate (PFDA), perfluorounde_x0002_canoate (PFUnDA) perfluorododecanoate (PFDoDA) and perfuorohexanesulfonate (PFHxS) 10.1021/acs.est.8b03030 legacy PFASs, known PFASs, and newly reported PFASs (emerging). In total 90 PFAS from 15 classes. 10.1021/acs.est.9b02211 na TFA PFPrA PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFHxDA PFOcDA TFMS PFEtS PFPrS PFBS PFPeS PFHxS PFHpS PFOS PFNS PFDS PFDoDS 4:2 FTSA 6:2 FTSA 8:2 FTSA na 10.1016/j.scitotenv.2019.133810 perfluorooctane sulfonate (PFOS), perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHxS), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluoro-1octanesulfonamide (FOSA), N-methylperfluoro- 1-octanesulfonamide (MeFOSA), Nethylperfluoro-1-octanesulfonamide (EtFOSA), 2(N-methylperfluoro1-octanesulfonamido)ethanol (MeFOSE), and 2-(N-ethylperfluoro-1octanesulfonamido)-ethanol (EtFOSE) 10.1155/2021/5564994 PFHxA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFOS, PFHxS PFTreA PFTriA PFDoA PFUnA PFDA PFOS PFNA PFecHS PFOA PFHxS PFHpA PFHxA PFBS PFPeA PFBA FHEA FOEA FDEA FOUEA FHpPA FHUEA 10.1039/d0em00510j PFBA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFBS PFHxS PFOS 6:2 FTS FOSA N-MeFOSE N-MeFOSA N-EtFOSE N-EtFOSA 10.1038/srep09859 10.5562/cca1776 10.1016/j.chroma.2011.01.085 PFCA analogues (CnF2n+1COOH, n=1-18) perfluorinated carboxylic acids (PFCAs PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUdA PFDoA PFTeDA PFHxDA PFODA PFBS PFHxS PFOS PFDS PFOSA 10.1016/j.chemosphere.2014.02.037 na 10.1016/j.wasman.2019.02.004 10.1016/j.envpol.2010.01.013 Polyvinyl fluoride (PFVF) Polyvinylidene fluoride (PVDF) Ethylene-terafluoethylene (ETFE) Perfluoroalkoxy (PFA) Perfluoroalkoxy (PCTFE) Fluorinated ethylene_x0002_propylene (FEP) PFBuS PFHxS PFHpS PFOS PFDS PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoA PFTrA PFTA FOSA N-MeFOSA N-EtFOSA 10.1016/j.jhazmat.2020.122493 10.1016/j.wasman.2016.08.024 PFBuS, PFHxA, PFOA, PFPeA, PFHpA, PFDeA, PFHxS na 10.1016/j.envpol.2009.12.031 PFBS PFHxS PFOS PFDS PFBA PFHxA PFHpA PFOA PFNA PFDA PfUnA PFOSA 10.1016/j.talanta.2013.02.020 PFHpA, PFOA, PFNA, PFOS, PFDA, PFUnA, PFDoA 10.1016/j.watres.2014.09.014 PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA 10.1016/j.chemosphere.2020.128018 11 PFCAs, 4 PFSAs, 3 FOSAs, 3 FOSAAs, 3 FTAs, 4 FTSs and 4 recent replacements of PFOS and PFOA 10.1016/j.chemosphere.2013.04.010 10.1021/acs.analchem.0c01591 PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFBS PFHxS PFOS MPFHxA M8PFOA M9PFNA M6PFDA M7PFUnDA MPFDoDA MPFHxS M8PFOS 27 PFAS 10.1016/j.scitotenv.2020.143944 51 PFAS - included nine PFSA(C3-C10, C12),and thirteen PFCA(C4-C14, C16, C18), twenty four perfluoroalkylated (PFAA) precursors (4:2, 6:2, 8:2 and 10:2 FTS; 6:2, 8:2 and 10:2 FTCA(FHEA, FOEA, FDEA, respectively); 8:2 and 10:2 FTUA (FOUEA, and FDUEA, respectively); 6:6 and 6:8 PFPi; 6:2, 8:2 and 6:2/8:2 diPAP, diSAmPAP; FBSA;FHxSA;N-AP-FHxSA;FOSA; NMeFOSA; N-EtFOSA; FOSAA; N-MeFOSAA; N- EtFOSAA), and five other PFAS (8Cl-PFOS; 6:2 and 8:2 Cl-PFESA (9Cl-PF3ONS and 11ClPF3OUdS, respectively); NaDONA; and PFECHS 10.1021/es1003846 na 10.1021/acs.est.9b07281 10.1021/acs.est.0c06690 The 25 target PFASs included 11 perfluorocarboxylic acids (PFCAs), seven perfluorosulfonic acids (PFSAs), three fluorotelomer sulfonic acids (FTSs), one perfluoroalkylsulfonamide (FOSA), two polyfluorosulfonamido acetic acid derivatives (NMeFOSAA and N-EtFOSAA), and perfluoro-2methyl-3-oxahexanoic acid (GenX). 10.1016/j.wasman.2018.11.035 10.1016/j.watres.2014.10.049 10.1016/j.wasman.2010.03.035 _PxF0O0S04_ fluorinated polymer PFDS PFOSA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA trichlorofluoromethane (CFC-11) and dichlorodifluoromethane (CFC-12), dichlorofluoromethane (HCFC-21), chlorodifluoromethane (HCFC-22), chlorofluoromethane (HCFC-31), difluoromethane (HFC-32), and fluoromethane (HFC-41) 10.1016/j.chemosphere.2020.128504 C4F8, CF4, C2F6 and other 10.1016/j.chemosphere.2016.08.112 PFPA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFBS, PFHxS, PFHpS, PFOS, PFDS 10.1016/j.chroma.2018.03.047 perfluoroether carboxylic acids (PFECAs) 10.1007/s00216-019-01829-8 53 PFAS from 14 compond classes (full list in article) 10.1016/j.chroma.2021.462369 water samples were spiked with PFAS in order to see if the method could detect them 10.1007/s00216-014-7689-8 [PFOS, PFOA, perfluoroheptanoic acid (PFHpA), perfluorohexanoic acid (PFHxA), perfluoropentanoic acid (PFPeA), perfluorobutanoic acid (PFBuA)] 10.1016/j.jhazmat.2014.03.016 PFAAs, including PFOA, PFOS, and the perfluorinated analogues: perfluorobutane sulfonic acid (PFBS), perfluorohexane sulfonic acid (PFHxS), perfluorooctane sulfonamide (PFOSA), perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnA), and perfluorododecanoic acid (PFDoA) 10.1016/j.watres.2016.02.055 PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFBS PFHxS PFOS 10.1021/acs.est.7b00315 (4:2, 6:2, 8:2, 10:2, 12:2, and 14:2 FTOH 10.1021/acs.est.0c08092 PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, 6:2 FTSA, GenX 10.1007/s10661-015-4425-6 perfluorohexane sulfonate (PFHxS) perfluoro-1-octanesulfonate (PFOS) perfluorodecane sulfonate (PFDS) perfluorooctane sulfonic acid (PFOSA) perfluorobutanoic acid (PFBA) perfluoropentanoic acid (PFPeA) perfluoro-n-hexanoic acid (PFHxA) perfluoro-n-heptanoic acid (PFHpA) perfluoronoctanoic acid (PFOA) perfluoro-n-nonanoic acid (PFNA) perfluoro-n-decanoic acid (PFDA) perfluoron-undecanoic acid (PFUnDA) perfluoron-dodecanoic acid (PFDoDA). 10.1016/j.chroma.2019.06.019 PFBA, PFOA, PFDA, PFOS 10.1016/j.scitotenv.2010.07.049 PFCs (PFBS, PFHxS, PFOS, 10.1007/s10661-012-2759-x PFBS PFHxS PFHpS PFOS PFDS PFOSA PFBA PFPA PFHxA PFHpA PFOA PFNA PFDA PFUDA PFDDA PFTrDA PFTeDA 10.1016/j.chemosphere.2020.129143 44 PFAS 10.1007/s00244-018-0585-z. 6:2 FTSAS 6:2 FTSAS-SO 8:2 FTSAS-SO 8:2 FTAB 10:2 FTAB 6:2 FtSaMAm 6:2 FtSa 4:2 FtSaAm 8:2 FtSaAm 5:3 FtB 7:3 FtB 9:3 FtB 5:1:2 FtB 7:1:2 FtB 9:1:2 FtB 6:2 FtTHN+ 8:2 FtTHN+ 6:2 FtTHN+-SO 8:2 FtTHN+-SO PFHxSAmA PFOSAm PFHxSAm FHxSA PFNS PFPeS 10.1016/j.chemosphere.2018.06.024 PFOA, PFOS, perfluorohexanoate (PFHxA), perfluoroheptanoate (PFHpA), perfluorononanoate (PFNA), perfluorodecanoate (PFDA), perfluoroundecanoate (PFUnDA) perfluorododecanoate, (PFDoDA) and, perfuorohexanesulfonate (PFHxS) 10.1016/j.envpol.2013.07.048 10.1016/j.chemosphere.2014.07.082 2 perfluorinated acids Perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnDA), perfluorododecanoic acid (PFDoDA), perfluorobutane sulfonic acid (PFBS), perfluorohexane sulfonic acid (PFHxS), perfluorooctane sulfonic acid (PFOS), perfluorodecane sulfonic acid (PFDS) and perfluorooctane sulfonamide (FOSA). 10.1016/j.heliyon.2019.e02315 10.1016/j.talanta.2017.08.052 53 PFAS: E.g. 11 PFCAs and 8 PFSAs Perfluorobutanesulphonic acid (PFBuS, CAS no. 375-73-5), per_x0002_fluoropentanoic acid (PFPeA, CAS no. 2706-90-3), perfluorohexanoic acid (PFHxA, CAS no. 307-24-4), perfluorohexanesulphonic acid (PFHxS, CAS no. 355-46-4), perfluoroheptanoic acid (PFHpA, CAS no. 375-85-9), perfluorooctanoic acid (PFOA, CAS no. 335-67-1), perfluoro-n-(1,2,3,4 13C4)octanoic acid (MPFOA), perfluoroactanesul_x0002_phonic acid (PFOS, CAS no. 1763-23-1), and perfluoro-1(1,2,3,4 13C4) octanesulphonate (MPFOS), perfluorononanoic acid (PFNA, CAS no. 375-95-1), perfluorodecanoic acid (PFDA, CAS no. 335-76-2) 10.1016/j.jhazmat.2020.122044 PFBS PFOS FBSA FOSA sum of PFAS 22 10.1021/es4044374 na 10.1016/j.scitotenv.2018.03.024 PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTriDA, PFTeDA, PFHxDA, PFOcDA, PFBS, PFHxS, PFOS, PFDS, FOSA, MeFOSA, EtFOSA, MeFOSE, EtFOSE, FOSAA, MeFOSAA, EtFOSAA and 6:2 fluorotelomersulfonate (FTSA) 10.1007/s11356-010-0335-x PFOA PFOS 10.1016/j.chroma.2017.08.001 10.1016/j.envint.2019.104982 PFHxA, PFDoDA, PFHxS, PFOA, PFOS 17 PFASs,: PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFHxDA PFODA PFBS PFHxS PFOS PFDS 10.1016/j.chroma.2014.05.003 10.1016/j.chroma.2016.10.060 10.1007/s00216-016-0110-z PFOA, PFNA, PFOS, Pentafluoropropionic acid fragment, PFBA, Perfluoropentanoic acid fragment, PFHpA, PFDA, Perfluoroundecanoic acid, Perfluoroundecanoic acid fragement PFOA, PFOS PFCA n:2-FTCA FTUCA PFPA PFSA FTS FASA FASE FTOH mono-PAP FASAA FTEOC 10.1016/j.chemosphere.2018.06.024 4:2 FtS 6:2 FtS 8:2 FtS FPePA FHUEA FOUEA FOSA MeFOSAA EtFOSAA PFBS PFHxS PFOS PFDS PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUA PFDoA CAS (if available in publication) Sampling written with the names 22 samples of eight representative types of bioresources were collected for investigation. These included land applied materials:biosolids(anaerobically digested sewage sludge) (n=3), CLO (n=2), MBMA (n=3) and PLA(n=3). Urban runoff samples were collected between November 2010 and March 2011 at sites around the San Francisco Bay (SF Bay), California. A total of 33 samples from 12 storms and 10 sites were analyzed. Samples were collected during the rise, na peak, and fall of the storm hydrograph. Effluent samples (n =12) were collected in duplicate from six STWs along three rivers. Runoff samples were collected from grass field drainage (n =3) and street runoff (n =2) during periods of rainfall. Grab samples were collected (200 mL) in amber glass bottles. All bottles were washed three times with 50/50 acetonitrile:acetone (v/v) followed by three washes with milli-Q water and were rinsed with sample water before collection. Water samples were collected from STW effluent outfalls and drainage pipes (both field and street) directly prior to entering the river flow. After collection, samples were stored at 4 C in the dark until vacuum filtration (within 8 h of collection) na using GF/F glass membrane filters. samples were collected from 18 landfills either directly from a valve after flushing, or using a polyethylene baler for leachate obtained from na manholes and ponds Air sampling was conducted above the aeration tanks of two WWTPs. At each site, a high volume samplers operated directly above the aeration tanks; prior to the sampling, cartridges for PFC analyses were spiked with 50 mL of an na internal standard solution Air samples were collected with a passive sampling technique using sorbent-impregnated polyurethane foam (SIP) disks. Plant leaves of local species were collected by precleaned na scissors. air and water samples from seven MSW disposal sites in china. All samples were collected in 500 mL glass or polyethylene jars, and to the best of our knowledge no Teflon containing tools were used during sampling of sludge; thus eliminating possible contamination during sampling of sludge samples by PFASs. Samples were collected from only processed sewage sludges intended for disposal. The biosolids composites analyzed in this study constitute a representative sample (94 na facilities) of the more than 16,000 U.S. WWTPs. Limed biosolids samples were collected from a large municipal WRRF in the Mid-Atlantic na region of the US Two deep gas probes were installed permanently in the center of waste cell 1.5.1 in order to sample and analyze the composition of the gas generated within the waste. Each gas probe had two individual screens ranging na from 2-3 m to 4-5 m below ground surface na na Sewage Sludge samples from 45 WWTPs in Switzerland between August and December (2011) in 3 sampling campaigns, with 3 samples collected from 21 plants, 2 samples from 22 plants and 2 samples from 1 plant. The interval between sampling events was of at least 1 month. Sites determination was selected based on the ocurrence of known or assumed PFAS related industrial and comercial activities. Samples of anaerobically stabilized sewage sludge (digested sludge) were collected (digested during 20-30 d). The water content of the digested sludge was na approximately 95%. surface water samples (5 L for each sampling point) were taken from the Oujiang River, at Wenzhou city, China the vicinity of where the discharge from a municipal WWTP enters the river. This WWTP is known to receive wastewater from the electroplating industry, where both F-53B and PFOS are assumed to be in use. Wastewater samples were also collected "upstream", at a small WWTP which treats the raw effluents of electroplating plants na before they enter the municipal sewer system. groundwater sampling in an area used to treat na raw sewage in Berlin. na waste water Groundwater samples were collected from thirteen shallow monitoring bores using a low flow pump with dedicated low-density poly ethylene (LDPE) tubing, into 250 mL polypropylene bottles. Sampling locations (n= 13) included sites installed directly in waste material and down-gradient from landfills, some of which exhibited na evidence of leachate contamination. Dust samples from e-waste dismantling areas, from communal flats near an industrial park, na from student dormitoreis MWWTP2 and MWWTP3) on six occasions in 1 year, i.e. once every 2 months. The MWWTPs treat mostly domestic water but also industrial wastewater (Table 1). In addition, a target industry's (metal plating) wastewater was sampled four times. Storm water, landfill leachate and municipal sewage sludge were sampled twice. Storm water was collected from the Porolahti creek, where the storm water sewage gathers urban runoff from an indus- trial area. The sampling times were November 2009 and April 2010. Landfill leachate was sampled from the equal- ising tank at mmssuo waste disposal site in October 2009 and June 2010. MWWTP3 sludge was sampled in January and June 2010. The wastewater of the target industry is treated in MWWTP3, and the landfill leachate in MWWTP2. All treated effluents are discharged into the Gulf of Finland except MWWTP1, which is discharged into the Archipelago Sea (Gulf of Bothnia). Wastewater and landfill leachate were collected as 24 h composite samples into high- density polyethylene containers. The MWWTP samples were adjusted to flow rate, and kept at +4 C during sampling. Landfill leachate and IWWTP1 sam- ples were adjusted for time (grab samples once an hour). The canisters were kept cold during the sampling. Storm water, sludge and target industry wastewater samples were taken as grab samples. The MWWTP sludge was sampled before digestion to plastic containers. Samples were transported to the laboratory within 24 h of sampling. Water samples were mixed and divided into bottles for various analyses (PFAA na samples in polypropylene bottles). 3 municipal waste water treatment plants. Sludge samples were collected as composite sam_x0002_ples during one day in October in the years 2012, 2014, and 2015 na from all three WWTPs. For each sampling point, water and sludge samples were collected and stored in high density, methanol rinsed, and air-dried polypropylene bottles. Water samples were prepared by centrifugation at 3,000 rpm for 10 min followed by filtration using 0.45-m nylon membranes, and stored at -20C until extraction. Sludge samples were dried in a freeze dryer and homogenized with a mortar na and pestle. six landfills were sampled and a total of seven leachate samples were collected. Two samples came from two different refuse cells in the same landfill (sites B1 and B2) and one sample came from na an evaporation pond (site F) Leachate (4L) was obtained April 13, 2010 from a Municipal Landfill A total of 128 groundwater samples were collected from thirty-eight shallow monitoring bores over five sampling campaigns in November 2015, May, June and August 2016 and May 2017 in Melbourne, Australia. Samples were collected using a low-flow bladder pump with dedicated low-density poly ethylene na (LDPE) tubing Biosolid samples were collected from16WWTPs located insix of na the eight states and territories of Australia six leachate samples were collected from four lined landfills in the US prior to leachate treatment. All samples were collected by grab methods involving either bailer, peristaltic pump, or collection from a tap. Leachates were collected in 125 mL polypropylene bottles from the landfills and shipped overnight on ice where na they remained frozen until analysis. Korea. 57 soil samples were collected from in- dustrial complexes (n=33), landfills (n=8), farmlands (n=4),woodlands (n=4), and mountains (n=8) in 2017. Industrialsampling sites were located within chemical (n=12), textile(n=6), na electronics (n=11), and metal (n=4). Samples taken from 10 Norwegian landfills between April and June 2018 Sediment samples were taken from na sedimentation pods of presten Flow proportional sampling was carried out during two- weekperiods in May, June, August, September na and October of 2019 Landfill leachate samples Leachate (n = 26), fly ash (n = 20), and bottom ash (n = 24) samples were collected from three MSW incineration plants (referred to as Plant A, Plant B, and Plant C) located in na Shenzhen, China In the supplementary data 2-5 samples of leachate-impacted groundwater were collected at each of 20 closed landfills in Canada Pretreatment and the ultimate disposal of leachate differed for each facility. Ultimate disposal at two landfill facilities consisted of on-site aeration with disposal to a WWTP. For two other landfill facilities, the leachate was discharged to a WWTP without on-site treatment. At one facility, the leachate was discharged to deep well injection without on- site treatment.Leachate was collected in two half-liter high density polyethylene (HDPE) bottles per sampling location. One collection bottle was used for subsequent PFAS analysis and the other was used to measure pH and chemical oxygen demand (COD). The purpose of these analyses was to define bulk physical- chemical characteristics as the leachates are na produced by different waste types. na na grab sewage sludge samples were collected from individual wastewater treatment plants, freshly digested sludge samples (approximately 500 g for each sample, wet weight, w.w.) from the WWTP dehydration process were packed in aluminum foil, sealed in polypropylene bags, and immediately express-delivered to our na laboratory Water samples were collected at each sampling site using Go-Flo bottles (General Oceanics Inc., Miami, Florida, USA) at a depth of 4-5 m. Go-Flo bottles avoid sample contamination at the surface, internal contamination, loss of sample on the deck, and exchange of water from different depths. Samples were stored at na 4 C in the dark before analysis. 375-22-4 2706-90-3 307-24-4 375-85-9 335-67-1 375-95-1 335-76-2 375-73-5 355-46-4 1763-23-1 Take samples as specified in DIN 38402-11, DIN 38402-12, DIN 38402-13, DIN 38402-15 and DIN ISO 5667-5 Use only cleaned vessels for sampling and fill them completely with the water sample 375-22-4 2706-90-3 307-24-4 375-85-9 335-67-1 375-95-1 335-76-2 375-73-5 355-46-4 1763-23-1 According to DIN 38402-24, DIN 38414-11, DIN EN ISO 5667-13 Leachate from WWTP was collected from the leachate lift station (a sump that collects leachate from the drainage layer of the landfill and perimeter ditches before it is pumped off site for treatment) using a stainless steel bailer na or a pump. Surface and raw wastewater samples were collected in high density polyethylene bottles na carefully cleaned with HPLC water and MeOH. na water (influent, effluent) Raw leachate grab samples (unfiltered, 2 L) were taken from the leachate lift station before the leachate was pumped off-site for treatment. Leachate treatment facilities at the study sites employed a two-stage process that integrated an external membrane bioreactor (MBR) unit with a post-treatment reverse osmosis (RO) or nanofiltration (NF) unit. Treated leachate samples (unfiltered, approximately 2 L of each sample type) including the bioreactor mixture, ultrafiltration (UF) effluent, NF effluent and RO effluent were taken during the treatment process as 24 h composites. All samples were collected in polyethylene (PE) bottles pre-washed with methanol. Samples were then stored at 4 C and extracted for anal- ysis within four weeks of sampling. PTFE (polytetrafluoroethylene)- based materials were avoided throughout the sampling and analysis to avoid potential na sample contamination leachates from 4 municipal solid waste landfill na sites na leachate Water samples from one of the largest fluorochemical industrial parks in China, located in Changshu, Jiangsu Province, near the Yangtze River. Influent and effluent samples were collected by peristaltic pump for 4 h from the WWTP of the fluorochemical industrial park. Three water samples each were collected from downstream of the YangtzeRiver near the WWTP and the Yangtze River in the Nanjing na section. Water samples were collected from various locations with known or suspected PFAS contamination for screening of ultra-short- chain PFAAs. Three different types of samples were collected at FFTS : outflowing water from rock shelter and groundwater before and after treatment with granular activated carbon na (GAC) filters. na na na na surface samples were taken from canals near textile dyeing, paper recycling workshops and na plastics recycling workshops 29420-49-3 3871-99-6 1763-23-1 375-22-4 2706-90-3 307-24-4 375-85-9 335-67-1 375-95-1 335-76-2 2058-94-8 307-55-1 72629-94-8 376-06-7 67584-42-3 812-70-4 70887-84-2 27854-31-5 53826-12-3) Grab samples are collected in polypropylene containers. Sample containers and contact surfaces with PTFE shall be avoided. Water, sediment and biota (polychaetes, pelagic zooplankton, crabs, fish, glaucous gulls) samples were collected from locations impacted by a firefighting training site (FFTS) na and a landfill as well as from a reference site; thermolysis products of na Nafion N117 in different temperature ranges. na 5 different sewage sludge samples (sludges 1- 5) were collected during April 2010 in a na domestic WWTP in Catalonia, Spain na na materials recovery from silicon-based PV modules. Representative samples of the polymers were taken from the PV module by manual removal na with a stylet wastewater, sludge, and sediment samples were collected in 3 different WWTP in Hong na Kong Eight raw and seventeen treated grab leachate samples after biolo-gical treatment with activated sludge process and/or advanced treat-ment with RO were collected na from eight landfills in Northern Greece sampling was done in 3 landfills with municipal waste solid and construction and demolition debris in Germany. Using to methods: grab cranes following na regular grid and drilling using no clear pattern. Untreated and treated landfill samples were collected in 250 mL polypropylene na (PP) bottles at 22 landfills sites in Germany. Dehydrated sewage sludge samples were obtained from dif- ferent waste-water treatment plants of La Rioja. The samples were frozen and protected from light. Spiked samples at a concentration level of 50 and 16 ng g--1 of each analyte were used to optimise the FUSLE conditions and to study the features of the method, respectively. These samples were prepared by adding an analyte standard solution in methanol and the mixture was thoroughly homoge- nised. Then, the samples were freeze-dried, ground and stored na in darkness at 4 1C. Sampling was conducted according to the Bureau of Sewerage, Tokyo Metropolitan Government (2012), the middle and downstream water reportedly consisted of approximately 50% STP effluents. The collected samples were decanted into methanol-rinsed 3 L high density polyethylene (HDPE) bottles and were kept in ice for up to 12 h. Upon arrival at the laboratory, the samples were stored at 4 C until analysis. Care was taken to avoid the na usage of any PTFEecoated materials. Samples of sewage treatment sludge were collected during a two- year sampling period (2018e2019) from 43 na different WWTPs located in the Czech Republic Sludge samples were collected from wastewater treatment plants and the respective sewage stabilization ponds in amber glass flasks in order to preserve the chemical composition of the samples, by protecting the samples from light, humidity and other external factors. The sludge samples had a water content of approximately 95%. Prior to extraction, the samples were air-dried, ground and homogenized by sieving through a stainless steel 2-mm sieve before extraction. When not undergoing extraction procedures, dried and sieved samples were stored in a na freezer at 20 C. Samples from landfill leachate collected from na an active MSW landfil in Florida US. The landfill soil (top 15 cm) was randomly collected down the slope of the landfill, from the working area (external to the top liner area) using a 3 m 3 m grid. Five subsamples (four corners plus the center) were taken and mixed to make one na homogenized composite soil sample soil samples were collected. The sampling equipment, composed of stainless steel, was washed three times with Optima-grade methanol (MeOH) prior to use. The samples were stored in certified-clean 500-mL, widemouth high-density polyethylene (HDPE) containers. The sampling equipment and containers were determined to be free of contamination for the intended analytes before the sampling trip by rinsing a representative of each item type with 60/40 (volume/volume) acetonitrile/ water (ACN/H2O) and analyzing the rinses. Surface-soil samples were collected from the 0- to 10-cm interval using sampling spoons, hand augers, and pans. Subsurface-soil samples were collected by Geo-probe from intervals bounded between the 23- to 56-cm and the 152- to 165-cm depths (Table SI1). na 17 PFAAs na waste waters at 3 positions Samples taken from a typical PV panel with polycrystalline na silicon wafers Septic water and tap water were collected from four dwellings at lakefront sites whereas lake water was collected along the shoreline of the residences from a deck, ~40 feet from the na lakeshore monofill shredder residue; the waste was sampled from a depth of 1-1.5 m below the surface. Large samples (75- 88 kg) were collected in an effort to reduce sampling error caused by heterogeneity of the waste and stored in 218 L steel drums sealed with airtight na lids. na Flue gas from semiconductor industry wastes of electrical & electronic equipment na (WEEE) collected at a sorting plant Fluorochemical contaminated water samples were acquired from North Carolina Department of Environmental Quality (NCDEQ) at a location near the industrial waste out fall for a local fluorochemical manufacturer, as well as from downstream drinking water treatment plants. Location 1 was the source water drawn from the Cape Fear River for a downstream water treatment facility and Location 2 was finished drinking water delivered to Wilmington, NC. Each sample was collected in a one liter HDPE bottle and stabilized by pH adjustment with nitric acid. Samples were stored at room temperature, extracted and na analyzed within five days of the sampling date. list of cas is wastewater, surface water, and included in article drinking water from Australia na Tap water and wastewater Effluent wastewater (n=6) and surface water (n=6) samples were collected from a wastewater treatment plant located in Seville (South of Spain) and from Guadalquivir na River (Seville, Spain) Raw influent (RI), primary effluent (PE), and final effluent (FE) samples were collected in 20 Canadian WWTP. Primary sludge (PS) was sampled from the underflow of the primary clarification tank and waste biological sludge (WBS) was collected from the underflow of the secondary clarification tank. Treated biosolid was sampled after the final treatment step. PS, WBS and biosolids were collected as grab samples. Wastewater and biosolids samples were sub-sampled into 1000 ml wide- mouth high-density polyethylene bottles and shipped to the laboratory on ice by na overnight courier. Single grab samples of treated final effluent were collected during peak diurnal flow in September and October 2014 from eight na WWTPs that discharge to SF Bay influent, secondary effluent, and sludge adn na mass flow samples of 12 municipal WWTPs na na Wastewater and sewage sludge from hospital and WWTPs were collected from six towns (Bungoma, Busia, Kakamega, Kisumu, Kisii, and Mumias) in Kenya that lie within the Lake Victoria basin in na January to March 2013 na na in 3 engineered landfils, leachates and na sediments were sampled. Water samples were collected from Hanoi city and its surrounding areas, Vietnam (dry season). The sampling locations in Hanoi included areas near a municipal dumping site and a municipal wastewater discharge station. Samples were also collected from creeks, rivers, and ponds at an e-waste recycling site (ER; Bui Dau, n010), a lead battery recycling site (BR;Dong Mai, n07), and a rural control site (RU;Duong Quang, n06) in Hung na Yen province Biosolids were collected from 19 participating WWTPs from three Australian na states wastewater from firefghting exercises, effluent from the WWTP, runnof water (RW), lagoon water and water used for diluting foam na concentrates (WFF), HDPE bottles influent, effluent and biosolids samples from na 14 WWTP Grab water samples were collected at the outlet of the WWTP Bitterfeld-Wolfen, na Saxony-Anhalt, Germany Influent water, effluent water and sewage sludge samples were collected from three WWTPs in three different na Swedish cities wastewater, surface water, CAS no in article and drinking water samples 375-73-5, 2706- 90-3, 307-24-4, 8 drinking waters (DW), 12 ground waters 355-46-4, 375-85- (GW), 13 surface waters (SW), 8 influents and 9, 335-67-1, 1763- 11 effluents of 23-1, 375-95-335- wastewater treatment plants (WWTPIN and 76-2 WWTPOUT) Biosolids samples were collected from twenty WWTPs in eight provinces across Canada. Grab samples were collected using stainless steel pails and stored in pre-cleaned amber glass jars (Systems Plus, Baden, ON, Canada). WWTPs consisted of five advanced treatment (AT) plants, twelve secondary treatment (ST) plants, and three primary treatment with chemical addition (PT) plants. Advanced treatment (AT) included biological nutrient removal processes, which removes nitrogen and phosphorous in addition to oxygen demand through a series of different na microbial environments. Flow-proportional effluent samples (24 h) were na collected from 10 WWTPs Wastewater, surface water, soil and plant samples, grab samples of wastewater were collected in duplicate from the influent and effluent of Bugolobi WWTP, surface water grab samples (50 cm below the water surface) were collected manually (using a rope and bucket) in duplicatestored in plastic bottles, which were pre-washed thoroughly with distilled water and ethanol prior to use; plant samples (yam roots, na maize cobs, sugarcane stems) Grab water samples were collected in spring from the municipal WWTP of Bayreuth. From 14 March to 18 May 2007, five grab water samples were collected from the WWTP (4250 mL) and the river (4500 mL) every other week on Wednesday (10:00 h, influent and primary treated waste waters). 48 h after the first sampling (duration of the waste water treatment process), samples of effluent of the WWTP and of river water, 0.1 km upstream and 1 km na downstream of the WWTP, were collected. imidazole ionic liquids immobilized on silica gel were synthesized through a chemical bonding method, and the immobilized dodecylimidazolium ionic liquid was selected as the receiving phase material in a POCIS (polar organic chemical integrative sampler) like passive sampler to monitor five perfluoroalkyl na substances (PFASs) in water Influent, effluent and excess sludge samples were collected from six WWTPs (W1-W6) along the Yanghe River during four sampling na campaigns na whoamteorgenates were packed into polyethylene bags and stored at -18 C as duplicate laboratory samples. After the freeze-drying procedure, solid samples were thoroughly homogenized and stored at +4 C prior to the analysis. Organic extracts of the samples were analyzed within three days of sample na preparation. effluent water sample from a municipal WWTP in Germany and 24-h composite influent sample and the corresponding 24-h composite effluent sample of an industrial WWTP in na Europe were collected and used in this study. na influent, midpoint, and effluent samples sample amount used Details in the Supplementary Information na na na na na na na 1L na na na 5 mL na na 250mL 200 mg na na na 1L 4L 250 mL leachate samples (50 mL), biosolifds( 0.5g) 125 mL 2-5 g freeze dried soil na 4L Grab samples (1 L) Leachate: 5 mL. Ash: 200 mg 200 ml 200 mL na na na na 1 0,01 g 4L na na na na na 1L 4L na na 1 L 5-mL sample size per analysis na na na na na 5mg na 2 ml composite samples were mixed into one 10L sample 250 mL na na 1 g sludge na na 5.0 g soil na organic composts na 110 g na na 300 ml air 1L na 250 ml 500 ml tap water or 200 ml waste water na 400 mL - 1000 mL 500ml- 1L na na na na 1 Liter 2 x 100L 0.5-1 g 250 mL na 20L na 250 mL na na na na WWTP (4250 mL) and the river (4500 mL) na inffluent and effluent: 4 L, 1L and 100 mL na na 1L na Pre- treatment Extraction Details in the Supplementary Information Details in the Supplementary Information solid phase extraction (SPE) (Oasis WAX SPE cartridges, 6 cm3 , 150 mg, 30 m; Waters, Milford, MA) as described by na Taniyasu et al.2 Membrane filters were soaked in 10% nitric acid for 12 h (to degrade any organic compounds within or on the filter) followed by three rinses under vacuum filtration with 50:50 acetonitrile:acetone (v/ v) and three rinses with HPLC water. Solid Phase Extraction (SPE) of 200 mL sample water was carried out using Phenomenex Strata-X cartridges preconditioned with 3 mL 50:50 acetonitrile/acetone (v/v), washed with 3 mL HPLC- grade H2O and loaded at a rate of 5 mL/min. Loaded cartridges were dried under vacuum for 15 min and eluted with 2 7 mL aliquots of 50:50 acetonitrile/acetone (v/v) at a rate of 1 mL/min. Extracts were evaporated to dryness using rotary evaporation and reconstituted with 1 mL of (80:20 HPLC H2O/acetonitrile, v/v) spiked with internal standards to 25 ng/mL. leachate samples were centrifuged, titrated to pH 7-8, and extracted with na trifluoroethanol and ethyl acetate. PUF/XAD-2/PUF cartridges were cold extracted three times (1 h, 1 h, 30 min) using methyl-tert butyl ether (MTBE)/acetone 1:1 (v:v). The extract volume was reduced to 150 mL by rotary evaporators and a gentle stream of nitrogen. Prior to the measurement, 50 mL of an injection standard solution containing 13C HCB and TCB D3 (c 400 pg mL--1) were added. Prior to the extraction of particle-phase PFCs, 50 mL of standard solutions containing 18O2 PFHxS, 13C PFOS, 13C PFBA, 13C PFHxA, 13C PFOA, 13C PFNA, 13C PFDA, 13C PFUnDA and 13C PFDoDA (c = 200 pg mL--1) were added to the filters. PFCs were extracted by fluidized bed extraction using methanol. The extract volume was reduced to 150 mL. Prior to the measurement, 50 mL of an injection standard (EtFOSAA D5 (c = 400 pg mL--1) na were added. at 15,000 g for 10 min. A 500 L supernatant was transferred into an auto- sampler vial before analyzed. Plant leaves: Leaf samples were purified by deionized water to remove the particulate matter on the surface, and then were processed with vacuum freeze drying technique. Then one gram of freeze-dried and homogenized leaves and 5 ng of each mass-labeled standard were added in a PP tube. For ionic PFASs, 5 mL of methanol was added and the mixture was sonicated for 30 min at 40 C. Then the tube was centrifuged at 4200 g for 10 min. This procedure was repeated once and the supernatants were combined. The combined extracts were cleaned up with GCB-Carbon cartridge and dried under a gentle stream of pure nitrogen to 500 L before being transferred into an auto- sampler vial. For neutral PFASs, 5 mL of 2 mM sodium hydroxide and 2 mL of ethyl acetate were added and the tube was shaken for 12 h in the dark and then centrifuged at 4200 g for 10 min. This procedure was repeated twice and the supernatants were combined. The combined extracts were dried by anhydrous sodium sulfate and further dried under a gentle stream of pure nitrogen to 500 L. Then the concentrate was cleaned up with 25 mg dispersive Envi- Carb (120/400 mesh, CNW Technologies, Germany) and centrifuged at 15,000 g for 10 min. A 100-L aliquot of the supernatant was transferred into an auto- na sampler vial before being analyzed. All information in the Supplementary Information All information in the Supplementary Information na EPA Method 1694 Solids from primary treatment as well as the secondary and nitrification treatment processes are thickened, combined, and dewatered through centrifugation. Lime is added to this sludge mixture on a dry weight basis of approximately 15e20% to neutralize pathogenic organisms, classifying the product as Class B biosolids All limed biosolids samples were extracted on a wet weight basis; extraction according to a referenced publication; samples were spiked with 15 ng of 13C5-PFPeA, 13C8PFOA, and 13C8-PFOS na na na na Dried sewage sludge samples (500 mg) were transferred into a 15 mL polypropylene tube. After addition of 0.5 mL water, the sludge samples were spiked with 40 mL of 0.5 ng /mL internal standard mixture of 13C4-PFBA, 13C2- PFHxA, 13C4-PFOA, 13C2-PFDA, 18O2PFHxS, 13C4-PFOS with an absolute amount of 20 ng per each compound. The samples were sequentially extracted three times with 2.5, The sewage sludge samples were dried at 40 C for 7-10 d 1.5, and 1.0 mL of methanol (Sun et al., (depending on the water content) in porcelain bowls, 2011a). Each extraction finely ground was performed by shaking the slurry for 10 (<0.5 mm) and stored in polyethylene bottles at room min, sonication for temperature. 20 min at 40 degrees C and centrifugation As the PFAAs were sorbed onto the sludge matrix. at 3500 rpm for 8 min. filtered through glass microfiber filters solid phase extraction (SPE) on-line-solid phase extraction na (SPE) na na Each 250 mL sample was filtered using glass fibre filters (1.2 mm,Millipore, Ireland) pre-rinsed with ultrapure water solid-phase extraction (SPE). air-dried and filtered MTBE 100 % methanol (MeOH), which was used to prevent the complex matrix of the leachates from getting into the extract. Both cartridge types were conditioned with 20 mL MeOH and 5 mL Milli-Q water. After the sam- ples were loaded, the Bond Elut Plexa cartridges were washed with 3 mL of 40 % MeOH (Aq), dried with a vacuum, and the analytes extracted with 3.0 mL of 1 % NH3 in MeOH. The WAX cartridges were washed with 2 mL of 2 % formic acid and 2 mL of MeOH, and the analytes were extracted with 3.0 mL of 1 % NH3 in MeOH. The extracts were cleaned with 100 mg activated carbon (Supelclean ENVI-Carb 120/400); 0.5 mL of ex- tract was diluted with 0.5 mL of Milli-Q water into a vial, and spiked with recovery standard (13C4-PFOA). Freeze-dried sewage sludge samples (1 g) were placed in a polypropylene tube and spiked with surrogate stand- ards and 200 mM NaOH solution. After the samples were soaked for 30 min, the analytes were extracted with methanol according to the method applied in the PERFORCE project (de Voogt et al. 2006). The method is based on studies by Powley et al. (2005). Methanol extraction was repeated twice for each sample. The extracts were combined, and evaporated to 1.0 mL with Personal Evaporator EZ-Envi (Genevac, Ipswich, UK). The extracts were purified with activated carbon. For LC-MS analysis, 0.5 mL of extract was diluted 1:1 with Milli-Q water and the recovery standard na 13C4-PFOA was added. The water samples were filtered with GF/B glass fiber filters before extraction (Whatman). SPE was performed using WAX sorbents according to ISO/DIS 25101 with some modifications na homogenized and centrifuged na The filtrated water samples were spiked with 5 ng of 13C8-PFOA and 13C4-PFOS as internal standards. The spiked samples were then loaded onto Oasis WAX cartridges preconditioned with 4 mL 0.1% NH4OH methanol solution and 4 mL MilliQ water sequentially. The flow rate was maintained at 1 drop/s through the cartridge. The cartridge was then cleaned up with 4 mL of 25 mmol/L sodium acetate buffer (pH 4) and dried completely under vacuum. The target compounds were eluted by 4 mL of 0.1% NH4OH methanol solution into a polypropylene tube and were concentrated under nitrogen to a final volume of 0.5 mL. The sludge samples: Dried samples of 0.5 g sludge was weighted into 15 mL polypropylene tube and soaked with 0.5 mL ionized water before spiked with 5 ng of 13C8-PFOA and 13C4- PFOS as internal standards. The sludge was extracted three times with 2.5, 1.5, and 1.0 mL of methanol. Each extraction was performed by shaking for 10 min, sonicating at 40C for 20 min and centrifuging at 3,500 rpm for 8 min. The extracts were combined, and 300 mg Envicarb particles was added directly into the extract and shaken gently for 20 min to clean up the extract. The solution was separated from Envicarb particles by centrifugation at 3,500 rpm for 30 min and concentrated under nitrogen to a final volume of 0.5 mL. micro-LLE was similar to that described by Backe et al. (2013) with adjustments. Unlike the method of Backe et al. (2013), no sodium chloride was added. Extractions were performed on unfiltered subsamples (3 50 mL) using solid-phase extraction (SPE) na na extracted twice with methanol, vortexed and centrifuged. Samples were further na extracted with a mixture of DCM: hexane. na solid-phase extraction soil samples were freeze-dried and mixed to obtain homogenous samples Methanol (sediment: centrifugation in methanol SPE-methanol Samples were initially collected in 2 LHDPE bottles and transported to the laboratory, where they weredivided into 250 mL aliquots in HDPE bottles and stored at18Cuntil analysis. H4OH in MeOH Samples were filtered through a 0.7 lm glass fiber filters (Whatman, England) before storage at 4 _x0003_C until extraction. Samples were extracted and concentrated before analysis using an AutoTrace 280 automated SPE system from Dionex Corporation, similar to previously published methods (Anumol et al., 2013) Leachate: supernatant was extracted using Leachate was centrifuged at 10,000 rpm for 15 min. Oasis WAX cartridges Ash: homogenized in a solvent cleaned pestle and mortar Ash: Methanol Samples were filtered (0.45-m polyethersulfone membranes) and preserved Solid phase extraction addition of internal standards that were isotopically labeled followed by a filtration step (Whatman GF/A glass fiber), and then followed by a solid phase extraction (SPE) process using Oasis WAX cartridges (Huset et al. 2011, Backe and Field 2012). Transfer of the samples from the sampling bottles used in the field to the filtration flask followed EPA standard protocols requiring volume measurement and a methanol rinse solid phase extraction (WAX Cartridges) na na samples were then lyophilized, homogenized, and preserved at -20 C until analysis, dispersive solid phase extraction (DSPE) method for the analysis of PFASs in environmental matrices na sample preparation protocol was based on the ISO 25101/2006 method Depending on the aqueous matrix, different volumes of water were extracted. In case of surface- and sewagewater, 50 mL water was extracted, while 250 mL was used for seawater samples. The 13Clabelled internal standards were supplemented to every sample prior to extraction to a final concentration of 100 ng L-1. Solid-phase extrac- tion was carried out using OASIS HLB cartridges (6 cm3, 200 mg, Waters, Milford, MA). The cartridges were pre-conditioned with 2 mL methanol and 2 mL Biosolve water. After loading, the car- tridges were rinsed with 2 mL Biosolve water for surface- and sewagewater. For seawater, 3 2 mL Biosolve water was applied. Subsequently, the cartridges were dried under vacuum for 10 min. Elution was achieved using 2 2 mL methanol. Next, extracts were concentrated to 0.5 mL under a gentle stream of nitrogen. Finally, 0.5 mL of 2.5 mM ammonium acetate in water was added before transfer to LC-MS vials. Samples were stored at 4 C before analysis. The samples are analysed in the unfiltered state. The pH WAX (weak anion exchange) value of the sample should lie in the range between pH 6 Solid Phase Extraction (Use at least 60 mg and pH 8 and shall be adjusted with sodium hydroxide of the solid phase material (7.3) for a solution or sulfuric acid, if necessary sample volume of e.g. 50 ml) When preparing the sample, observe the specifications of the Sewage Sludge Ordinance (AbfKlrV) and the Federal Soil Protection Ordinance (BBodSchV). A sufficiently homogeneous laboratory sample must be available for taking a partial sample (test sample). Observe the specifications according to DIN 19747 for taking partial samples. The sample must not be dehydrated before homogenization, e.g. by centrifugation, as the soluble fraction of some PFCs cannot be neglected. Homogenize water sediments and thin-bodied sewage sludges by stirring and take a subsample, if necessary with continued stirring. For soil, compost, pressed sludge and animal feed, reduce laboratory sample according to DIN 19747, e.g. by means of cross-rugation divider (8.6). Sort out foreign materials and record gravimetrically; if necessary, examine these materials separately. Take a partial sample and dry it; measure the partial sample in such a way that, if possible, at least a dry mass of 5 g can be expected. The subsample must be representative of the laboratory sample and, for soil samples, should be at least 1/4 of the mass of the laboratory sample. In the case of homogeneous, fine-grained and free-flowing materials, the subsample may be less. Preferably freeze-dry sewage sludge according to DIN 38414-22 (8.5), other samples if necessary at 40 C in a drying oven, depending on the water content. Translated with www.DeepL.com/Translator (free version) Sonication with MeOH 50-mL subsamples (n = 3/time point) were adjusted to pH 7 using ammonium hydroxide and then spiked with isotopically labeled internal standards. Oasis WAX cartridges (Waters, 150 mg, 6 cc) were preconditioned with 5 mL of 0.1% ammonium hydroxide in MeOH, followed by 5 mL of MeOH and 5 mL of Millipore water prior to use. Samples were loaded at a rate of 1 drop/second, and then cartridges were washed with 5 mL of 0.1% ammonium hydroxide in water. PFASs were eluted with 14 mL of acetonitrile (ACN), followed by 5 mL of 0.1% ammonium hydroxide in MeOH, and the na eluants were combined. Samples of 250 mL of wastewater were successively passed through 2.6mm and 0.3mm glass-fiber (GF/F) membrane filters using a Nalgene filtration unit. Extraction of the suspended particulate matter (SPM) was conducted according to a sediment extraction procedure adapted from Bertin et al. . Briefly, filters were sonicated twice with 5 mL of MeOH (20 min). Extracts were cleaned-up with graphite (0.25 g), and evaporated to dryness under a N2 flow and moderate heating (40 C). After reconstitution in 250mL of a 20 ng mL-1 internal standard solution in EtOAc, extracts were sonicated, vortexed and a 200mL aliquot was transferred to a 1.5 mL glass vial. The extraction of the wastewater filtrate was conducted as follows: Strata X-AW cartridges were conditioned with 8 mL of MeOH/ NH4OH 0.2% in water (v/v) and 2 4 mL of HPLC water. After sample loading, cartridges were rinsed with 5 mL of HPLC water, dried for 1 h under vacuum, and centrifuged (3 min, 5000 rpm). Analytes were recovered with 2 4 mL of MeOH/NH4OH 0.2% in water (v/v), the eluates being directly passed through graphite cartridges (coconut charcoal, 2 g) previously conditioned with 10 mL of MeOH. Extracts were finally evaporated to dryness and reconstituted in 250mL of a 20 ng mL-1 na internal standard solution in EtOAc. na SPE-methanol The raw and treated leachate samples were centrifuged at 11,000 g for 15 min to remove large particles before extraction. The amount of PFAAs absorbed onto particles (except for the bioreactor mixture) was considered low because of the small amount of particles (less than 200 mg L-1) present in the leachate. After centrifugation, the supernatants of leachate samples were spiked with internal standards prior to extraction using a solid phase extraction (SPE) method. The supernatant and solid sludge from the bioreactor mixture were analyzed separately. Sludge samples were further air-dried and extracted according to a method developed in our previous study (Li et al., 2010), which includes sonication solvent extraction, SPE and dispersive na carbon sorbent cleanup. filtered with 0.7 mm fiberglass filters (GFF, ChmLab) to eliminate particulate matter. An aliquot of 70 mL of each leachate sample was spiked in duplicate with IS MPFAC-MXA (30 ng of each analyte, see Table S1) prior to solid phase extraction (SPE) in order to correct losses and matrix na effect Following measurement of pH, samples (50 mL) were adjusted to approximately pH 7 with hydrochloric acid, spiked with 10 ng of M8-PFOA and M8-PFOS and shaken to mix. Samples were loaded onto HLB or Strata-X cartridges (pre-conditioned with dichloromethane (DCM), methanol and MilliQ water) at a rate <10 mL per minute. Cartridges were dried under vacuum, and then eluted with 2 mL acetone, 7 mL methanol followed by 6 mL of DCM. The eluent was concentrated to approximately 1 mL under N2 and transferred for further clean up onto pre-conditioned Supelco Envi_x0002_carb cartridges (250 mg; 3 mL) using methanol. Cartridges were eluted with acetone (2 mL), methanol (6 mL) and DCM (5 mL). Samples were concentrated to 1 mL, transferred to a glass vial and spiked with 10 ng of the labelled recovery standard (MPFAC-MXA) for LCMS/MS na analysis. 250 mL of influent and 500 mL of effluent were separately used for solid- na phase extraction. filtered water samples were extracted by weak anion-exchange solid-phase extraction (WAX-SPE) following the ISO25101 method with some na modifications. were extracted using a method modified from ref na 50 mL aliquots were loaded onto Oasis WAX cartridges (6 mL/150 mg, Waters) at 1 drop/s. Samples were spiked with known quantities of internal standards (M8PFOS, M8PFOA, M8FOSA, MPFHxS, MPFNA, d-N- MeFOSA, d-N-EtFOSA (Wellington Laboratories)). The cartridges were dried under vacuum for 30 min, and eluted with 4 mL methanol, followed by 5 mL methanol (0.1% NH4OH). Eluents were concentrated at 35 C under a gentle stream of nitrogen to ca. 0.5 mL and loaded onto an ENVI-carb (3 mL/250 mg, Sigma Aldrich) SPE cartridge. PFAS were eluted with 2 mL methanol (0.1% NH4OH) and concentrated to 200 L containing 10 ng of MPFOS (Wellington Laboratories) na and transferred to inserted LC vials. Water quality--Determination of perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA)--method for unfiltered samples using solid phase extraction and liquid chromatography/mass spectrometry" - ISO na 25101 : 2009 Standards and samples shall be in a 50:50 methanol:water solution containing 0.1 % acetic acid. Direct Injection Polychaetes were depurated overnight in seawater in order to separate sediment-bound PFAS from accumulated PFAS. Sediment and biota samples were extracted with methanol. Water and melted snow samples were extracted on Oasis Waters (Mildford, MA, USA) weakanion exchange (WAX) SPE cartridges (6 mL volume, 0.5 g). na na na na pressurized solvent extraction was carried na out in a PSE 240V na na thermal treatments at 600C no extraction but elimination was the goal dried at 105 C overnight and ground befor being homogenized by a solvent-rinsed blender. Waste water samples: Extracted based on a slightly modified version of the method (liquid solvent extraction) reported by So et al. (2004). Modifications: larger Oasis HLB extraction cartridges (0.5 g) were used rather than the 0.2 g cartridges used in the previous study, as high concentrations of PFC were expected. For sediments and sludges: modified version of the method proposed by Powley et al. (2005) was used (methanol extraction, supernatant acidification and pre-concentration). samples were filtered through pre-ashed glass-fiberfilters na Solid-phase Extraction na solid-phase extraction (SPE) as described elsewhere (Taniyasu et al., 2005; Ahrens et na al., 2009b) with a few modifications. A SONOPLUS 2070 focused ultrasound system (20 kHz, 70 W) equipped with a MS73 titanium microtip was used. 0.5 g of sample was placed with 8 mL of acetonitrile in a 34-mm glass tube and internal standards (M8PFOA and MPFOS) were added. Then FUSLE was performed twice for 20 s, at a pulsation of 0.5 and 65% of power. Extractions were carried out at 0 1C in an ice-water bath. After the extraction step, FUSLE extract was centrifuged for 5 min at 3000 rpm using an Orto Alresa Digicen centrifuge. The sample was washed twice with 4 mL of solvent each. Rinses were added to the extract and it was evaporated to dryness under a nitrogen stream using a Turbo Vap II concentrator (Zymark, Hopkinton, MA, USA). The residue was reconstituted in 2 mL of LC-MS grade methanol and extracts were filtered through a 0.2 mm nylon filter before the UPLC-MS/ na MS analysis. 125 mL unfiltered water samples were transferred to 125 mL HDPE bottles. One sample from each site was subsampled in triplicate (n = 3) and was added with 2 g (60 mM) of potassium persulfate and 1.9 mL of 10 N NaOH (150 mM). The HDPE bottles were placed in a temperature controlled oil bath (Personal He10 SH; TAITEC, Saitama, Japan) at 85 C for 6 h. Then, the samples were cooled to room temperature in an ice bath prior to analysis. The pH of the samples was adjusted between 5 and 9 by concentrated HCl prior to the extraction. Isotope labeled surrogate standards, 4 ng were added to the samples and blanks prior to the extraction in order to correct their recovery rates for each batch analysis. The collected sludge samples were freeze-dried, thoroughly homogenized Solid-phase extraction (SPE) nPaart of the samples (n 3)were concentrated in the lab with sintered glass aquarium air stones used to produce bubble air and to produce substancial foaming. The foam was collected for analysis. The other part of the samples (n=3) had no pretreatment. 1 g sample sludge was spiked with 1 ng mass labeled Internal Standard (IS) and transferred to a 50 mL polypropylene vial and extracted first with 4 mL 1% acetic acid in MeOH with sonication for 15 min followed by extraction with 4 mL 50/50 v/v MeOH and AcN, each time, the supernatant was collected. The combined extracts were then dried using a gentle stream of N2 gas before dilution with HPLC grade water for SPE extraction (using Oasis WAX cartridges (Waters, 6 cc/150 mg)). The elute from SPE was dried by passing a gentle stream of N2 gas, and subsequently reconstituted using 1:1 volume ratio of MeOH and Ammonium acetate solution to a volume of 200 lL, a procedure which involved addition of recovery internal standard, to make the final volume of 200 lL. na To obtain a homogeneous matrix, the thawed soil sample in the container was manually mixed twice (gloves were worn), each session lasting 5 min. 2 methods: Methanol or acetonitrile (they were equally good) sieved through a MeOH- washed, 2-mm, stainless-steel sieve and extracted in triplicate na ENVI-Carb cleanup extracted in triplicate using a method described by Choi et al. (2019) na thermal degradation at 500C na na na na anlosoexetlruatcetdiownitbhut5emlimL oinfamtieotnhwanaoslthe goal containing 0.1% ammonia. The eluents were combined and concentrated to ~500 mL under a gentle stream of nitrogen at 35 C using a TurboVap Evaporator (Zymark, Inc., Hopkinton, MA, USA). The final volume of the extract was adjusted to one milliliter in an amber glass vial, and 10 mL of the extract was injected into HPLC-MS/ MS for the analyses of PPCPs and PFASs. na na samples were cut and dried extracted with methanol with the addition of ammonium acetate (final concentration 5 mM) using warm Soxhlet extraction na SPE Samples were filtered using1-m glass fiber filters Solid-phase Extraction na Solid phase extraction Samples were filtered through a 1.2-m glass-fiber membrane filter (Whatman, Mainstone, UK), and the I.S. were added to achieve concentrations of 1 g /L Solid-phase extraction vortexing, centrifuged and filtered Solid phase extraction (SPE) oxidized for indirect measurement of PFAA pre_x0002_cursors according to a previously developed method (Houtz and Sedlak, 2012; Houtz et al., 2013) concentrating them with solid phase extraction (SPE) (Oasis WAX SPE cartridges, 3 cm3 , 60 mg, 30 mm; Waters, Milford, MA) For FTOH analysis in sludge, 0.5 g dw of freeze-dried samples spiked with 50 L of D4-4:2 FTOH (10 g/L), 13C2D2-6:2 FTOH (10 g/L), 13C2D2-8:2 FTOH (10 g/L), and 13C2D2-10:2 FTOH (10 g/L) was added to 15 mL PP centrifuge tubes. The samples were left to stand for 24 h at room temperature in the dark, and then 4 mL of ACN was added for extraction. After shaking for 20 min at 300 rpm and sonication for 20 min (40 C), the extract was separated by centrifugation at 4000 rpm for 10 min. One milliliter of the extract was diluted with 4 mL of ultrapure water and then loaded on WAX cartridges which had been conditioned by 3 mL of ACN and 3 mL of ultrapure water. Then, 200 L of DCM containing 30 mg/mL DNS and 30 mg/mL DMAP was added to the eluate, which was then shaken vigorously for 1 min. The resulting mixture was kept at 65 C for 60 min, and then 3 mL of ultrapure water and 6 mL of hexane were added. After 10 min of shaking at 300 rpm, the organic layer was separated by centrifugation at 4000 rpm for 10 min. The extraction process was repeated twice, and the combined extracts were loaded onto silica cartridges conditioned with 8 mL of DCM and 8 mL of hexane. The dansylated FTOHs were eluted with 8 mL of hexane:DCM (v/v, 1:1), blown to dryness, and then dissolved in 0.2 mL of na ACN for UPLC-MS/MS analysis. na MeOH sludge samples were dried in an oven at 105 C to constant weight (typically 24 h) and the water loss was determined gravimetrically. The dried samples were then ground and homogenized by sieving through a stainless steel 2-mm sieve before extraction. Dried and sieved samples were stored in a freezer at -20 C. Sludge extraction: Methanol and internal standards were adedd and vortex mixed, sonicated and centrifuged. Supernatants were transfered and extraction was repeated. Supernatants were concentrated and dried under nitrogen stream. water samples: Water samples were extracted by SPE with Oasis WAX cartridges (Waters, 6 cc/150 mg) as described by Taniyasu et al. (2005) and Orata et al. (2009). 50 mL of trichloro(1H,1H,2H,2H- perfluorooctyl)silane was dissolved in 50 mL of hexane. Scraps of paper (60 40 mm, length width) were immersed in the above solution for 5 min in an ultrasonic bath at room temperature for fluoro- functionalization. The fluoro-functionalized paper was then washed withn- hexane,methanol,methanol + water (1 + 1, v/v), and methanol successively in an ultrasonic bath and was dried at 60C. Pieces of the fluoro-functionalized paper (600 mg, cut to 3 4 mm, length width) and 100 mL of water sample were put into a centrifuge tube. The tube was retained shaken for 1 h on a water bath thermostatic oscillator at room temperature. The paper was picked out from the solution by a tweezer and then washed with water to remove impurities adsorbed on the paper surface by non fluorous-fluorous interaction. The PFCs adsorbed on the fluoro functionalized paper were desorbed in 2 mL of acetonitrile under ultrasonication for 5 min. The desorption step was repeated three times. The combined desorption solution was dried using a N2 stream. The residue was redissolved in 1 mL of acetonitrile. The sample solution was then filtered through a 0.7-m membrane, and 10 mL of the na filtrate was injected in a HPLC-MS/MS. About 2 g of dry sample was spiked with 20 L internal standard, 13C PFOS and 13C PFOA (0.5 ng/ L). 1 mL of 200 mM NaOH in methanol was added and soaked for 30 min. Then, 100 L 2 M HCl in methanol was added followed by another 9 mL of methanol. The mixture was thoroughly mixed and then extracted on a wrist- action-shaker for 30 min. After centrifugation (2000 rpm, 5 min), 1 mL of supernatant methanol extract was treated with 25 mg ENVI-Carb mixed in 50 L glacial acetic acid. After thorough mixing and centrifugation (10,000 rpm, 10 min), 20 L recovery standard, 0.1 ng/L 3,5- is(trifluoromethyl)phenyl acetic acid, and 0.5 mL of 4 mM NH4 OAc in water were na added to the final extract mixing in methanol Solid-phase extraction was carried out as described by Taniyasu et al. (2005) with minor modifications Prior to analyses, samples were freeze dried and homogenised to afine powderusing a ceramic homogeniser Methanol nonfiltered water samples (250 mL) were spiked with labeled internal standards and concentrated by solid phase extraction (SPE); Offline enrichment was conducted on an automated system. PFASs were eluted from the cartridges by the successive use of 1 mL of methanol (MeOH), 4 mL of ammonium hydroxide (0.1% (v/v) (NH4OH) in MeOH, and 2 mL of NH4OH 0.1% (v/v) in isopropanol/dichloromethane (30/70) before being combined and concentrated under a nitrogen stream to a fnal volume na of 100 L Water: samples were adjusted to pH 7 and loaded onto HLB or Strata-X cartridges and spiked with the internal standard (10 ng of M8-PFOA and M8-PFOS). Cartridges were dried under vacuum, and then eluted with 2 mL acetone, 6 mL methanol followed by 5 mL of DCM. The eluent was further cleaned up on Supelco Envicarb cartridges (250 mg; 3 mL). Samples were concentrated to 1 mL, transferred to a glass vial and spiked with 10 ng of the labelled recovery standard (MPFAC-MXA) for LC-MS/MS analysis. Biosolid sub-samples from each site were freeze dried, ground to a fine powder and pooled equally by weight before accelerated solvent extraction. Florisil (5 g) and biosolid samples (0.25 g) were weighed into 100mL stainless steel ASE cells and filled with hydromatrix. Cells were spiked with the internal standard (10 ng of M8- PFOA and M8-PFOS) and then extracted using three cycles of methanol and DCM (2:1). The extracts were transferred to a round bottomed flask and concentrated to approximately 1mL on a rotary evaporator. Concentrated extracts were subjected to further clean up on Envicarb cartridges (250 mg; 3 mL) using methanol. Cartridges were eluted with acetone (2 mL), methanol (6 mL) and DCM (5 mL). Samples were concentrated to 1 mL, spiked with the recovery standard (10 ng of MPFAC-MXA) and transferred to a na vial for LC-MS/MS analysis. solid-phase extracted (SPE) with 4 g of Chromabond HR-X sorbent (MachereyeNagel) in Omnifit columns na (Diba Industries Ltd.) dried at 105 degrees C and homogenized. with methanol, briefly votex mixed, sonicated, centrieuged and again extracted with methanol. Supernatants concentrated under nitrogen stream at 40 degrees C. na Solid phase extraction na na air dried and grounded with 60 mesh sieve. The sample preparation and extraction method has been described by Chu and Letcher, 2017; Chu et al., 2016, with some modifications: The sample was spiked with internal standards and ultrasonicated and extracted three times by 4 mL 0.2 % formic acid in ACN solution each time at 60 C. The extracts were combined, concentrated to 2 mL and diluted by 8 mL water. The diluted extract was cleaned up and fractioned by Oasis WAX SPE cartridges (60 mg 3 cc, Waters Limited, ON, Canada). A sample volume of 0.25 L was adjusted to pH 6.5 with formic acid or ammonia and pressure-filtered through a 0.7 m glass fiber filter (Whatman). Isotope-labeled IS (103 total, 100 ng, details in the SI) were spiked to each sample prior to enrichment with mixed-bed multilayer solid-phase extraction cartridges comprising Oasis HLB, Isolute ENV+, Strata-X-AW, and Strata-X- CW (exact details in Kern et al.19) via vacuum extraction at 10 mL/ min. The analytes were then extracted from the dried cartridges with a 6 mL basic (2% of 25% ammonia) followed by a 3 mL acidic mixture (1.7% of 100% formic acid) of ethyl acetate/methanol (50:50 V/V). The neutral combined extract was concentrated to 100 L under a gentle nitrogen stream, adjusted to 1 mL with HPLC-grade water, filtered through a 0.45 m regenerated cellulose filter into a 2 mL vial and stored na at 4 C prior to analysis. and then 4 mL of Millipore water, the cartridges were loaded with 500 mL of water sample at a flow rate of one drop per second. After percolation, the cartridges were washed with 4 mL of 25 mM ammonium acetate buffer (pH 4) in Millipore-water and centrifuged at 3000 rpm for 2 min. The PFASs were then eluted from the cartridges with 4 mL of methanol, followed by 4 mL of 0.1% ammonium hydroxide in methanol. The samples were concentrated to 1 mL under a gentle nitrogen stream and transferred to brown amber vials for instrumental analysis. For extraction of solid and plant samples, 3 g of each of the pooled samples were weighed into a 50 mL PP-tube and 2 mL of a 100 mM sodium hydroxide in methanol/ Millipore water solution (80/20, v/v) were added. The mixture was left to stand for 30 min and then 20 mL of methanol and 100 L of IS mixture (c = 20 pg L-1) were added. The mixture was shaken in a wrist- action shaker for 60 min at 200 rpm and centrifuged at 3000 rpm for 5 min. The supernatant was then decanted into a new PP-tube. This procedure was repeated once again by adding 10 mL of methanol to the original PPtube, shaking for 30 min at 200 rpm and centrifuging at 3000 rpm for 5 min. The supernatant was then decanted into the new PP-tube, 0.1 mL of 4 M hydrochloric acid was added and the tube was shaken by hand and centrifuged at 3000 rpm for 5 min. The sample wasconcentrated under a nitrogen stream na to 1 mL. Particulate matter was removed by centrifugation Solid-phase extraction (SPE) was done as described (Becker et al. 2008), modified as follows: to waste water 250 L of a 100g/L mixture of 13C-PFOA and 13C-PFOS each, to river water 100 L of a 10-g/L mixture of 13C-PFOA and PFOS each was added. Each IIL sampler was rinsed with distilled water to remove the materials adhering to the membrane surfaces and then vacuum freeze-dried. Then, the sampler was disassembled, and the IIL-silica gel or HLB sorbent powder was transferred carefully into an all-glass syringe (3 cc) previously blocked with glass fibre cotton on the bottom. Additional glass fibre cotton was pressed tightly on the powder. After that, the sorbent powder was eluted with 6 mL of elution agent (methanol containing 5% ammonium hydroxide). Procedural blanks were performed by pretreating the unused sor- bents (IILs and HLB) in the same process as the samples, and were examined together with samples to control for potential contami- nation from laboratory materials and solvents. For PFASs in the active sampling water samples, 500 mL water samples were filtered by 0.45 m cellulose nitrate membrane fil- ters before a WAX-SPE na process. wastewater samples: pretreated by filtering. Excess sludge samples were ground with ceramic mortars and pestles after being completely dried and then filtered through 0.15-mm nylon sieves prior to extraction. solid-phase extraction (SPE) based on methods previously reported by Chen et al. (2018) and Yuan et al. (2014). solid phase extraction (SPE) step using polymeric cartridges (Oasis HLB) with 200 na fmoLr 1o0f wmaintearts3a0m0p0lerplomadaendd the obtained methanolic extracts were transferred to a 50 mL graduated glass volumetric flask, diluted with reagent grade water to 50 mL, 50 _x0002_L of formic acid was added to each sample and the samples were applied to the SPE cartridges for pre-concentration na and clean-up. na sold-phase extraction Samples were stored up to 5 days at the WWTP at 4 C, transported to the laboratory, and analyzed and extracted within 2 days of receipt. Due to the concentrated nature of the samples, they were analyzed for target PFASs without preconcentration in a 50:50 methanol sample mixture amended with a surrogate standard stock solution used for quantitation with isotope dilution. Aliquots were taken an inch below the water level na after samples were gently agitated. Clean up Measurement Quantification method Details in the Supplementary Information Details in the Supplementary Details in the Supplementary Information Information rinsed with 4 mL of HPLC-grade water and dried under vacuum for approximately 1 h HPLC coupled with an Agilent 6410 triple quadrupole mass spectrometer operating in negative electrospray ionization mode. isotopically labeled surrogate standards na HPLC-MS/MS internal standard na LC/MS/MS internal standard neutral and ionic PFC was performed by na GC-MS and HPLC-MS/MS internal standard The 16 ionizable PFASs were analyzed using HPLC-MS/MS (Agilent Technologies, U.S.A.) and the 7 neutral PFASs were na analyzed using GC-MS internal standard All information in the Supplementary Information GC-MS internal standard EPA Method 1694 EPA Method 1694 na sample loading, cartridges were conditioned with 10 mL of ACN:MeOH (50:50 v/v). Extracts were loaded and collected. Car- tridges were washed with 3 mL of MeOH. This wash was also collected. Eluates were concentrated to 4 mL under a gentle stream of nitrogen, diluted in 175 mL of organic-free water, and acidified to a pH of approximately 4 using formic acid. Diluted and acidified samples were loaded onto Oasis WAX (500 mg, 6 mL) SPE cartridges (Waters, Milford, MA, USA) at a rate of one drop per five seconds. Cartridges were previously conditioned with 10 mL of MeOH and 10 mL of organic-free water. After sample loading, car- tridges were washed with 2.5 mL of 0.01% formic acid in MeOH. Compounds were then eluted and collected with two 10 mL washes of 0.5% NH4OH in MeOH. Sample extracts were analyzed via HPLC- MS/MS to measure for PFAS compounds using a Waters 2690XE separations module (Waters Corporation, Milford, MA, USA) attached to a Quattro Ul- tima benchtop triple quadrupole mass spectrometer (Micromass Limited, Manchester, UK) with an electrospray interface. Chro- matographic separation was obtained by injecting 10 mL of extract onto a Zorbax C8 (150 4.6 mm) reversedphase liquid chromatography column inline with a 4.6 12.5 mm guard column (Agilent, Santa Clara, CA, USA) at a temperature of 40 C (Powley et al., 2005). The mobile phase consisted of (A) 2 mM ammonium acetate in organic-free water and (B) MeOH and was run at a flow of 0.5 mL/min. The mass spectrometer source parameters were: capillary voltage 3.10 kV in electrospray negative (ES-); extractor voltage 1 V; RF lens 0.1 V; source temperature 140 C; desolvation temperature 400 C. Nitrogen was used as both the nebulizer (145 L/h) des- olvation gas (450 L/h). Acquisition was done in the multiple- reaction monitoring mode (MRM). Peak integration and quantitation were performed automatically using MassLynx4.0 (Micromass Limited, Manchester, UK). via MS with internal standard 13C5-PFPeA, 13C8-PFOA, and 13C8- PFOS prior to extraction as surrogate spikes and 13C5-PFHxA, 13C5-PFNA, and 13C3- PFHxS na GC-MS na na na na clean-up was performed according to (DIN 3841414, 2011) The combined extracts were enriched by solidphase extraction (SPE) on a Strata-X-AW cartridge Liquid chromatography tandem high resolution mass spectrometry (LC-MS/MS) Calibration standards (n = 7) were prepared in methanol with a final nominal concentration ranging from 0.1 to 300 ng /L of standard mix solution (from 0.1 to 100 ng /L for PFCAs and 0.5 to 300 ng/ L for PFSAs extracts were reduced using a gentle stream of nitrogen, diluted to 1 mL with ultrapure water and filtered LC-MS/MS, ZORBAX Eclipse XDB C18 column (5 m 2.1 mm 150 mm, Agilent, CA) using an UltiMate 3000 HPLC (Dionex by Thermo Fisher Scientific Inc., MA), API 3200 triple quadrupole mass spectrometer (AB SCIEX, ON, Canada) Potassium L-PFOS and 13C4- and 13C8-labeled L-PFOS, as recovery and injection standards na UPLC-HRMS na LC-QTOF-MS standards na liquid chromatograph (LC) coupled with an Agilent technologies 6495B tandem mass spectrometer (MS/MS) in negative na electrospray ionisation mode (ESI) analytical standards extraction was repeated with MTBE HPLC-MS/MS Internal standard na UPLC-MS-MS internal standard wash with 4 mL sodium acetate (NaAc) buffer solution (pH 4), followed by 4 mL of 20% methanol. Ultra Performance Liquid Chromatography (UPLC) system coupled to a triple quadruple mass spectrometer XEVO TQ-S (Waters Corporation, Milford, USA), in negative electrospray ionization mode Quantification of PFCAs, PFSAs, FTCA/FTUCAs, FTSAs, monoPAPs, diPAPs, and FOSA/FOSEs was performed by isotope dilution with masslabeled internal standards. na HPLC-MS-MS internal standard Isotopically-labeled na orthogonal LC-MS/MS internal standards na HPLC-MS/MS characterized isomeric mixtures of PFOS and PFOA, isotopically labeled internal standards (ISs; Table S1) and six point calibration curves. PC Titrator (alkalinity), dual column gas chromatography with flame ionization detector (dissolved methane), and inductively coupled na plasma mass spectrometry (cations). na AB/Sciex API 5500Q mass spectrometer (AB/Sciex, Concord, Ontario, Canada) coupled to a Shimadzu details of PFASs analysis Nexera HPLC system (Shi_x0002_madzu described in Galen et al., na Corp., Kyoto, Japan) w 2014 dispersive-carbon sorbent cleanup liquid chromatography/tandem mass spectrometry (LC/MS/MS) internal standards. Cartridge was washed with 6 mL of 25 mM ammoniumacetate HPLC-MS/MS Internal standard ENVI-carb clean-up UPLC-MS/MS. Internal standard na UPLC-MS/MS. internal standard Liquid chromatography and Mass spectrometry Leachate: cartridges washed using 4 mL of ammonium acetate buffer LC-MS/MS internal standard na UHPLC-MS/MS internal standard Methanol na Internal standard na na na na HRMS; API na na LC-ToF-MS internal standard Concentrate the eluate to dryness, e.g. in a nitrogen stream. Dissolve the residue in e.g. 1 ml using a mixture of solvent and water in accordance with the composition of the reference solutions. If necessary, filter the extract through a syringe filter and use a partial volume for the analysis. LC-MS/MS Calibration using a external or internal standard SPE WAX (optional) Elution with MeOH 0.1% NH3 HPLC-ESI(-)-MS/MS External and internal stan na HPLC-MS/MS Quantification was based on isotope dilution when an exact isotopically labeled standard was available (10 PFASs), otherwise an internal standard approach was used. na LDTD/APCI-Orbitrap-MS internal standard (APCI) combined with GC-MS/MS with triple quadrupole analyzer GC- (APCI)QTOF MS GC-(EI) MS and GC-(CI) GC-(APCI) MS MS SPE HPLC-MS/MS na 100 mg of EnviCarb activated carbon and 50 mL of glacial acetic acid were added in a centrifuge tube and vortex mixed along with the sample extract for 30 s. Centrifugation was carried out at 11000 rpm and extracts were then filtered (0.22 mm) and transferred to a 15 mL PP tube to be further evaporated until dryness under a gentle stream of dry nitrogen gas. The final volume was adjusted to 200 mL of Milli-Q water:methanol (70:30 v/v) prior to injection HPLC-QqQ MS/MS quadrupole Quattro Micro triple internal standard na LC-MS/MS na High-performance liquid Chromatography and high-resolution hybrid QTOF mass spectrometer (Triple TOF 5600, AB SCIEX, Foster City, CA, U.S.A.) operated with a negative PFASs standards and na electrospray ionization (ESI-). internal standards Mass labelled internal standards and recovery na SFC-MS/MS, UPLC/MS-MS standards The TOP assay is an indirect method for semi_x0002_quantifying PFAA precursors by oxidizing and converting precursors to measurable PFAAs. uPLC- na QToF/MS Analysis. na na HPLC-TOF MS internal standard the target compounds in the cartridge were eluted with 4mL of MeOH and 4mL of 0.1% ammonia solution LC/MS/MS with negative electrospray ionizationinterface internal standard na LC/MS/MS Internal & external standard (at a minimum, five calibration levels are required when using a linear calibration curve and six calibration levels are required when using a quadratic calibration curve.) Clean-up of methanol extracts was conducted using active carbon (EnviCarb, Sigma_x0002_Aldrich Co., PA, USA) The quantitative determination of PFAS was done with high-performance liquid chromatography (HPLC) using an Agilent 1200 series HPLC (Agilent Technologies, Waldbronn, Germany) and an Agilent 6460 (Agilent Technologies, Santa Clara, CA, USA) triple quadrupole mass spectrometer equipped with a jet stream electrospray ion source internal standard calibration curves with eight concentration points na LC/ESI-MS/MS) na na na na na LC-ESI-MS/MS. internal standards na na na gas chromatography-mass spectrometry na (GC-MS) analysis. ENVI-Carb UPLC/MS/MS PFC standards 6 mL of Milli-Q water were used for rinsing LC-HRMS/MS internal standard na according to standard EN 12457-4 na na Extraction cells were filled inserting two cellulose filters at the bottom of the cell, 1 g of anhydrous sodium sulphate and the sample were added and the cell was completely filled with anhydrous sodium sulphate. Finally, a cellulose filter was placed on top. Methanol was used as extraction solvent, and the PLE conditions were those reported by Llorca et al. [11]: a temperature of 70C at 100 bar and two extraction cycles of 1 min. After the extraction step, PLE extracts (ca. 15 mL) were evaporated to 0.5 mL under a nitrogen stream using a Turbo Vap II concentrator (Zymark, Hopkinton, MA, USA). The residue was reconstituted up to 2 mL of LC-MS grade methanol. Extracts were filtered through a 0.2 mm nylon filter before the UPLC-MS/MS analysis. HPLC-MS/MS UPLC-MS/MS using 20 internal standards Quantification was performed by multiple reaction monitoring (MRM) and ion extraction SPE HPLC-MS-MS Methanol LC-MS/MS na internal standard na UHPLC-MS-MS internal standard liquid chromatography (LC)-high- through 25 labeled resolution tandem mass standards (13C or 2 na spectrometry (HRMS/MS) H labeled) Two post-extraction cleanup strategies (ENVI- Carb and ion-pair). UPLC-MS/MS. internal standard Acetonitrile/water extracts were analyzed on a Waters Acquity ultraperformance liquid chromatograph (UPLC) interfaced with a Waters Quattro Premier XE tandem mass spectrometer operated in negative na electrospray-ionization mode. ba na na total oxidizable precursor (TOP) assay LC-QTOF LC-HRMS on orbitrap (targeted and untargeted) na HPLC-MS non-targeted na GC analysis with a classical thermal conductivity detector and a flame na ionization detector (GC/TCD/FI na na HPLC-MS-MS isotop dilution/ external calibration curve na GC-MS na GC-MS na mass spectra Concentrated extracts were filtered using a syringe filter (nylon membrane, 13 mm diameter and 0.45 mm pore size). The filtrate was concentrated using a stream of nitrogen in a TurboVap II (Caliper LifeSciences, USA) concentrator unit to 500 mL and transferred to a minivial. samples were diluted using a solution of ammonium ace- tate in water (concentration 5 mM) up to a final volume (50/50, ammonium acetate in water/ammonium acetate in methanol, v/v). Prior to final analysis, syringe standards (13C4 PFOA, 13C4 PFOS) were added to all samples. HPLC-ESI-MS/MS Internal standard na LC-MS/MS internal standard na LC-MS/MS 5 L of water was added to rinse cartridge LC-MS/MS Internal standard internal standard PFOA-13C8 High-performance liquid chromatography- were used as internal na mass spectrometry standards washed using 5 ml of reagent water followed by 5 ml of a solution containing 50% methanol and 50% 0.1 M formic acid in water. The cartridges were eluted with 4 ml of methanolic ammonium hydroxide (0.3%) (LC/MS/MS) standard solution containing 13C4-PFBA, 13C2-PFHxA, 13C2-PFOA, 13C5-PFNA, 13C2-PFDA, 13C2-PFDoA and 13C4-PFOS na UPLC-MS/MS analytical standards of PFASs and their stableisotope surrogates na dansylation UPLC- ESI-MS/MS method internal standard the cartridges were washed with 4 mL buffer solution 25 mmol L-1 acetic acid/ammonium acetate (pH=4) and centrifuged at 3000 r min-1 for 3 min to remove residual water UPLC-MS/MS. internal standard Quantification of the PFAAs was achieved using the internal standard method and a six-point external calibration curve covering a UPLC-MS/MS using electrospray ionization concentration range operated in negative ion mode according from the individual to a method method detection limits published in detail earlier (Vestergren et (MDLs) to 2.5 pg /L na al. 2012) na Fp-SPE-HPLC-MS/MS na na HPLC/MS system na ACQUITYTM ultra-performance liquid chromatography system (Waters, USA) coupled with a Quattro MicroTM API triple quadrupole mass spectrometer (MS/MS, Waters, na USA) in negative ionization mode na na LC-MS/MS internal standard PFASs were eluted from the cartridges by the successive use of 1 mL of metha-nol (MeOH), 4 mL of ammonium hydroxid UPLC-QTRAP/MS internal standard na LC-MS/MS washing with 400 mL of bidistilled water/methanol (90:10; liquid chromatographyehigh resolution v:v) mass spectrometry (LCeHRMS) internal standard Target com_x0002_pounds were quantified by standard addition, pentobarbital and the suspect seco_x0002_barbital by isotope dilution transfered to tubes with graphitized carbon and acetic acid, samples were again mixed and centrifuged. UPLC/MS/MS Acquity ultra- performance liquid chromatography system coupled to a Xevo TQ-S tandem mass spectrometer (UPLC/MS/MS; Waters Corp., Milford, MA) operated in negative electrospray ionization mode SPE cartridges were eluted using 2 mL MeOH that was used to rinse the sample bottle, followed by4mLof0.1%(v/v) ammonium hydroxide in methanol. LC-MS/MS Internal standard Ultra-high performance liquid na chromatographic (UHPLC) na UHPLC-MS/MS Non-isotopically labelled and labelled PFAS standard solutions were used. na HPLC-MS-MS internal standard prepared 1.7 mL Eppendorf centrifuge tube with 25 mg ENVICarb and 50 L glacial acetic, the supernatant was then filtered through a 25 mm syringe filter ( = 0.45 m) with a polypropylene membrane HPLC-EIS-MS/MS internal standard For calibration, a stock solution of 98 mg/L 13C- PFOA was prepared by dissolving 10 mg of 13C-PFOA (98%) in 100 mL acetonitrile, a 13C-PFOS (free acid) stock solution of 1.9 mg/L was prepared by diluting 1 mL of a 50-mg/L_x0002_solution 13C-PFOS sodium salt in a 25-mL PP-volumetric flask (Supelco, na LC-ESI-MS/MS (Weremiuk et al. 2006) Bellefonte, USA). All five PFASs were analysed with a 1200 Infinity series liquid chromatograph equipment coupled to a 6410 B triple- quadrupole mass analyser (MS/MS) with an electrospray ionization (ESI) source na (Agilent Technologies). na high performance liquid chromatography (HPLC) System coupled to an Agilent 6460 Triple Quadrupole LC/MS System (Agilent Technology, Palo Alto, CA, USA) with the negative electrospray ionization (ESI) na mode na na LC-TOFMS na SPE HPLC-Orbitrap-MS na HPLC-MS/MS-a (for analytes with acidic characteristics) cleaned with 3 mL H2O- HPLC-MS/MS-n (for analytes with neutral MeOH characteristics) internal standards SPE WAX (optional) Elution with MeOH 0.1% NH3 LC-QTOF, LC-MS/MS na WAsorking range (ng/mL) Matrices Reported levels (ng/mL) info - validation of the method Details in the Supplementary Information biosolids Sum of the 9 PFAS: 99-231 Details in the Supplementary g/kg in biosolids Information Urban Runoff: prio to oxidative treatment: PFOS (2.6-26 ng/L), PFOA (2.1-16 ng/L), and The PFAA precursor oxidation PFHxA (0.9-9.7 ng/L) method was validated with experiments using representative after oxidative treatment: C8 and C6 PFAA precursors: FOSA, N- PFCAs with 5-12 EtFOSAA, NMeFOSAA, 8:2 FtS, 8:2 diPAP, membered perfluoroalkyl 6:2 FtS, and 6:2 diPAP. The chains increased by a concentrations of precursors used in median of 69%, or control experiments ranged from 25 ng/L na na between 2.8 and 56 ng/L. to 25 g/L . na na na na na na na blank samples 97 to 1004 pg m--3 na na (neutral PFCs) na na 0.5 - 200 ng/l PFASs in the two landfills were up to 9.5 ng/m3 in the air, 4.1 g/g in dry deposition, and 48 g/g lipid in leaves with trifluoroacetic acid and perfluoropropionic acid being dominant (71% na -94%) na air, leachate 0.20 - 1.6 pg/m3 for air samples and n.d. - 6.2 ng/ L for leachate During the sample pretreatment, one procedural blank was per-formed and analyzed along with each batch of ten samples. On sampleinjections, instrumental blanks were run for every ten samples to mon-itor carryover effects na na na na From these analyzed compounds, the highest mean concentrations observed over the study period were 25.1 ng/g dw, 23.5 ng/g dw, and 22.5 ng/g dw for perfluorononanoic acid (PFNA), perfluorooctanoic acid (PFOA), and perfluorooctanesulfonic acid (PFOS), respectively, and these compounds were detected at Instrument detection limits (IDLs) were concentrations 2.5e5 determined as outlined by the USEPA times higher than the (USEPA, 1984) and the limit of remaining, detectable quantitation (LOQ) was established as na biosolids PFASs three times the IDL. gas contained different fluorocarbons: 27 micro g/ L . other results found on na na Table 1 na na na na na Accuracy was determined by spike and recovery experiments. The precision of the entire method, as indicated by the relative standard deviation was determined by extracting 3 replicates of the spiked sewage sludge. Relative recoveries ranged in general PFAAs (C4-C8) ranging between 80% and 120%, with the from 4 to exception of PFBS (65-95%). 2480 micro g/ kg; Recoveries of PFNA and PFDA varied Sewage PFOS ( predominant strongly and thus these sludge PFAA) 4 - 2440 mg/ kg compounds were only included in the samples (median 75 micro g/ kg); analysis if recoveries ranged from 45 from 80% to 120%. Procedural blanks WWTPs in PFOS median were tested with quartz sand Switzerland concentration of 82 micro that went through the whole procedure, near g /kg- 2290 mg/kg. including drying. A blind potential value of 0.04 lg kg_x0003_1 could be industrial PFCAs: up to 233micro g/ determined for only one compound, na emitters. kg. PFHxS. waste water (effluent 43-78 and 65-112 g/L and for the effluent and average recovery was 100.1% with na influent) influent, respectively relative standard deviation of <10% hindered determination due to elevated blank na na values. na na na na na The sum of detected field reagent blank (FRB), method blank PFAS (14PFAS): 26 ng/L - (MB), laboratory control sample 5,200 ng/L. (LCS) and two sites were selected by PFHxS : 2.6 - 280 ng/L . random number generator to PFOS : 1.3 - 4,800 ng/L. be sampled and analysed in triplicate. PFHxA: <LOQ - 46 ng/L. Statistical Analysis (ANOVA) was used to na na PFOA: 1.7 - 74 ng/L. analyse significance. values in dust: Legacy PFASs: 1,8 - 132 ng/g PFAS precursors: 0.6 - 7 ng/g All values highest from Quantification was performed by a 10point calibra-tion curve with a na dust industrial aera concentration range of 0.10 - 100 ng/mL. 1 - 7.9E+6 na na na Calibration curves consisting of at least five points were prepared for the targeted compounds. Procedure blanks treated in the same way as the samples were included in each batch of 8-10 samples. The method limit of detection (LOD) was determined as three times the signal in the procedural blanks, and in absence of the analyte in the blank, the lowest point in the calibration curve. Triplicates of three sludge samples from the WWTPs were used to assess the accuracy, precision, matrix effects, PFAS total concentration and recoveries of the na na in ranes from 29.8-77 ng/L method PFOA was the predominant PFCs in water phase, and its concentrations were in the range between 20 and 170 ng/L in influents and between 30 and 145 ng/L in effluents. PFOS and PFOA were the predominant PFCs in sludge samples, and their concentrations were 42- water, 169 and 12-68 g/kg, na sludge respectively. na Whole method precision was determined as the combination of inter and intraday variability and calculated using a one-way ANOVA . Estimated method detection limits (EMDLs) were defined as 3 times the S/N on either side concentration per PFAS in of analyte peaks in leachate na na table 2 extract Method accuracy averaged 119% for Reported only presence of target PFCs many different isomers in and 104% for ISs. Precision ranged from less time than other 4 to 19% RSD for targets and na methods. 2 to 7% RSD for ISs Statistical analisis ANOVA and Shapiro PFOA levels ranging from Wilk test to analyse significant na na 2.1 to 74 ng/L differences. To assess the reproducibility/precision of the extraction and analysis methods over time, an aliquot of a bulk biosolid or leachate sample was extracted and analysed with PFHxA: 12-5700 ng/L each batch of samples, as landfil PFHpA: 2.2-3500 ng/L a QAQC sample. Replicate and biosolids, PFOA :19-2100 ng/ L procedural blank samples were also na leacheates PFOS: (37-1100 ng/L extracted. Perfluoroalkyl carboxylates were the most abundant (67 4% on a nanomolar (nM) basis), up to 2,800 ng /L. Perfluoroalkyl sulfonates (22 2%) on a nM basis. Perfluorobutane sulfonate concentrations were as high as 2,300 ng/L. Sulfonamide derivatives composed 8 2.1% (nM The precision of the method, as basis) indicated by relative standard deviation (RSD) was determined by replicate Fluorotelomer sulfonates extractions (n=3) of a single leachate (6:2 and 8:2) composed sample. RSDs ranged na na 2.4 1.3% (nM basis) from 2 to 26% The sum 15 PFAS concentrations in soil from 0.175 to 11.7 ng/g. Soil from industrial complexes (0.346e11.7 ng/g), Landfills (0.504e10.4 ng/g: Soil samples from industrial areas, 15 PFAS concentrations from 3.11 to 11.7 ng/g, from the textile industries, 3.26e8.74 ng/g, from the metal industries, The PFAS concentrations quantitated by internal standard methodwere within the calibration range (0.05e50 ng/mL), and the cor-relation coefficients of the calibration curves were higher than 0.99for all curves. The relative standard deviations of the relativeresponse factors of each compound in the calibration na soil 1.53e5.71 ng/g solutionswere all below15% PFAS leachate concentrations ranged from 68 to 6800 ng/L water and Sediment_ 8.5-2120 ug/ na sediment l na mean total concentration of the 34 PFAS was 21131 ng/L The highest S34PFAS concentrations were (262 ng/L), and the lowest (172 Water ng/L) (leachate and we found that 34PFAS precipation only accounted for 12% runoff from 4% of EOF detected in PFASs were quantified by internal calibration using na the plant) the leachate corre-sponding mass-labelled standards. PFOA: 180- 2500 ng /L in all samples; PFOS: (<5-92 ng/ L in 2 samples. Five quality assurance and quality control (QA/QC) samples were included for analysis. They included a 1L ultrapure water blank, a laboratory control sample (LCS) using ultrapure water spiked with 300 ng L_x0003_1 of analytes and three matrix spike (MS) samples (Site A, Site B and Site D Tank) each spiked with 300 ng L_x0003_1 of analyte Procedural blanks were prepared at an interval of every six to eight samples to determine if contamination had occurred during sample extraction. Solvent blanks containing methanol and calibration check standards were Sum of PFAS prepared to run after every eight Leachate: 21.4-682 ng/mL samples to monitor the background Leachate, fly Fly ash: 1.46-87 ng/g contamination. Calibration curves were ash, bottom Bottom ash: 3.12-77.4 ng/ constructed using a series of PFAS na ash g concentrations The maximum individual PFAS concentration was for PFECHS (per- fluoroethylcyclohexanesul fonate), at 9.5mg/L, while PFOS and PFOAreached 2.7 and 0.85mg/L, respectively. The three landfills withmarkedly higher concentrations of PFAS, specifically PFSA, than theother sampling All analytes were quantified using a areas (i.e., DC-A, DC-B, 16-level calibration curve ranging from DC-C; maximumS17PFAS 0.01 to 15 ng/ml, R2>0.99. Quantitation of2.4e12.7mg/L;Fig. 1B) was based on relative response to the were all within the same corresponding isotopically labeled city, with disposallimited standard to correct for recovery and na water to the early 1960s matrix effects na na na na investigatio n-derived na waste na na na na na na PFOS was detected in every sample in levels up to 38.9 ng L-1, while PFOSA was found once at a concentration of 26.4 ng L-1. PFHxS and PFOA Besides the validation procedure of the were frequently detected accredited lab of the Flemish up to concentrations of Environment Agency (FEA), the 13.1 and 23.5 ng L-1, SANCO/2007/3131 document [22] was respectively. also used as guideline for the validation na na (Antwerp). of this new analytical method. The lower limit of application is 0,01 g/l, or 0,025 g/l for treated waste water. Water na The recovery rates of the internal standards are a measure of the analyte recovery over the whole analytical process, for each individual sample. They shall be determined in accordance with and shall lie in a range between 50 % and 150 %. Soil calibration from 10 Sediment g/kg to 500 g/kg Sludge na recovery of internal standards have to be PFAS concentrations in flow-through leachate (landfill A) ranged from 3.8 to 36 g/L and on a molar basis were made up of 31-71% PFAAs (15-56% PFCAs, 12-21% PFSAs) and 29-69% PFAA- precursors (19-48% FOSAMs, 9- 24% FTAs). Recirculated leachate (landfill B) generally contained lower PFAS concentrations (2.5 g/L), made up almost entirely assessment of method accuracy and of PFAAs (83% PFCAs and 17% PFSAs on a precision using triplicate spike/recovery experiments (10 ng of individual PFASs molar basis). spiked into 50 mL of recirculated landfill PFPeA and PFHxA were leachate and extracted along with na leachates the major PFASs detected. samples) can be found elsewhere PFOA and PFNA were quantified in all samples (range: 0.19-0.72 and 0.07-0.21 ng L-1, respectively) and PFDA in all samples but one (range:<0.02-0.25 ng L-1), while long-chain PFASs conducted on a filtered fresh influent na water were not detected. wastewater matrix na na 1.5 - 67 pg/mL na Regarding raw leachate samples, the total concentration of 11 PFAAs (PFAAs) ranged from 7280 ng L-1 (CZ) to 292,000 ng L-1 (SH), with a mean value of 82,100 ng recovery of internal standards have to be na na L-1. 50 % bis 150 % Total PFASs ( PFASs) in raw leachates reached 1378.9 ng/L, while in treated samples PFASs was approximately two- fold (3162.3 ng/L). PFCAs accounted for the majority of the detected PFASs and perfluorooctanoic acid (PFOA) was the dominant compound in raw leachates (42.6%), followed by shorter chain PFHxA (30.1%), PFPeA and na leachate PFBA na Five PFASs were detected ubiquitously, with perfluorohexanoate (PFHxA) the predominant PFAS (mean 1700 ng/L; na leachate range 73-25,000 ng/L). na 0.1, 0.5, 1 ng/L, 0.5ppb influent and effluent na (only mentioned in %) blank samples ; sensitivity of instrument analysis for four different levels of known PFAS standard solutions were used for verification; spiking of procedural recovery with 0.5 ng fg known PFAS standards to check recovery method. . Ultra-short-chain PFAAs were detected in all samples at concentrations up to 84 000 ng/L (C1-C3), representing up to 69% of the concentration of 29 per- and polyfluoroalkyl substances (PFASs). Trifluoroacetic acid (TFA), perfluoropropanoic acid (PFPrA), trifluoromethane sulfonic acid (TFMS), perfluoroethane sulfonic acid (PFEtS), and perfluoropropane sulfonic acid (PFPrS) were detected at concentrations up to 14 000, 53 000, 940, 1700, and 15 000 ng/L, na na respectively. blank samples PFAA loads ranged from 28.7 to 75.9 g/kg for OFMSW composts that included food packaging and from 2.38 to 7.60 g/kg for composts that compost did not include food na material packaging na respect to PFASs, the predominant compounds were: PFBS (arithmetic mean = 1100 ng L-1) PFOA (790 ng L-1) PFOS (270 ng L-1) MilliQ sample spiked with target PFHxS (200 ng L-1) compounds was also analysed with each na leachate PFNA (30 ng L-1) batch of samples (n = 4). metal-plating factories: 0.73-18.91 textile-dyeing factories: PFOA and/or PFHxA, which were present in all effluent wastewater samples,varied from 0.37 Six-pointcalibration curves were to 15.96 ng/L and 1.07 to developed for each target analyte 43.58 ng/L, respectively bydiluting calibration stock in methanol surface water samples of at concentrationsranging from 0.5 to na na craft villages: 0.83 to 58.2 20ng/mL. 10 - 400 ng/L, 50 - 2000 ng/L for PFPeA, PFBA, 200 - 8000 ng/L for FDEA, 300 - 8000 ng/L for FOEA, FHEA na Water Sludge Influent Effluent Wastewater Water, sediment and biota This test method was tested by CRL on reagent water. was 643 84 ng L-1, while it was 365 8.0 ng L-1 in a freshwater pond and 57 4.0 ng L-1 in a creek in the vicinity of the FFTS. These levels were an order of magnitude higher than in coastal seawater of the nearby fjord (maximum level PFAS = 10.1 1.2 ng L-1, at the FFTS impacted site). PFOS was the most predominant compound in all seawater samples and in freshly fallen snow (63-93% of PFAS). In freshwater samples from the Longyear river and the reference site, PFCA C9 were the predominant PFAS (37-59%), indicating that both local point sources and diffuse sources contributed to the exposure of the marine food web in the fjord. PFAS concentrations increased from zooplankton (1.1 0.32 g kg-1 ww) to polychaete (2.8 0.80 g kg-1 ww), crab (2.9 0.70 g kg-1 ww whole-body), fish liver (5.4 0.87 g kg-1 ww), and gull liver (62.2 11.2 g kg-1). The recovery limits for the RLCS are 35 to 150 %, if any analytes are outside of these limits the QC failure is explained in a narrative accompanying the data. full validation carried out not reported, only na na reported presence. na na na na na (PFOS): 53.0 - 121.1 microg/kg. validated using an "in-house" procedure Oder PFCs: 0.3 and 30.3 according to ISO 11843 using spiked na na micro g/kg materials bec na na na na mechanical removal of the backsheet from the PV panel allows to eliminate the formation of HF, COF2 and fluorinated na na organic compounds na instrument detection limit (IDL) was set at three times the standard deviation of the Waste water PFOS: 19.0 background levels detected in the to 49.9 ng/L blanks, and the method detection limit (MDL) was in sludge and sediments: calculated based on the IDL according to PFOS: less than 100 ng/g U.S. EPA na na PFDS: not detected guidance (Gomez-Taylor et al., 2003) The quantification of the detected contaminants was based on thestandard addition method, while a Screening Raw leachate: LOD - 14,7 Detection Limit (SDL) isprovided for the g/l non-detected analytes. The SDL is not compound-specific, but a generic Treated leachate: LOD - reporting value derived after method na water 15 g/l validation. na na na na treated and untreated leachates in different WWT processes. na In untreated leachate: sum of PFC concentrations ranged from 31 to 12,819 ng/L. The dominating compounds were PFBA (mean contribution 27%), PFBS (24%), PFHxA (15%), PFOA (12%), PFPA (6.0%), PFHpA (4.0%), 6:2 FTS (3.7%), PFOS (2.7%), and PFHxS (2.3%). in treated leachate: sum of PFC concentrations ranged from 4-8060 ng/L . Almost all target compounds were detected (39 of 43 PFCs) Quality control and assurance included the using of 20 internal standards, recovery rates, method blanks, mass detection limits (MDL), mass quantification limits (MQL), control standards, reproducibility and the calculation of the matrix effect na na <3.03 ng/g na The concentration of the 15 PFAA and 3 PFAA precursors before oxidation in the river water samples were 3.8- na na 38 ng L--1 . na PFAS contamination of sewage sludge, reaching values from 5.6 to 963.2 ng /g . PFOS was the most Sludge abundant among the (freeze- targeted PFAS, reaching na dryed) 932.9 ng g1 na quantified perfluoroalkyl carboxylates and perfluoroalkyl sulfonates concentrations ranged from 10 to 597 and 14 to na na n54o0reppgo/grt,erdesvpaelucteisv.ely na comments: 19 of 27 PFAS were significantly higher in the foam compared to na na the unadultered leachate na na (can be found in the can be found in the na soil supplementary na na isotopes highest concentrations were perfluorodecanoic acid (990 ng/g), perfluorododecanoic acid (530 ng/g), perfluorooctanoic acid (320 ng/g), and perfluorooctane sulfonate na (410 ng/g) na biosolids biosolid-based products (9.0 - 199 g/kg) > food and yard waste (18.5 g/kg) > other 27 organic products (0.1 - 1.1 g/kg). PFBS was quantified at the highest concentration among the samples (8040 ng L-1) The sum concentrations of the target PFASs in the diluted discharge samples from each fab were 623, 394, and 376 ng L-1 sum concentrations of target and nontarget PFASs in the diluted discharge samples from each fab were 1490, 78 700, and na waste water 2170 ng L-1 na proposed treatment lies in the total elimination of the emissions of hydrofluoric acid and fluorinated organic compounds deriving from the Tedlar na na degradation na na na 0.20 to 14.6 na na na na na mass spectrum and GC retention times na flue gas 3.32-6.21 ppmv of C4H8 were used to idenify C4H8 wastes of electrical & electronic equipment WEEE materials contained (WEEE) PFOS in the range of 0.07 collected at - 0.43 mg kg--1 and also a sorting other PFASs and PFCAs at Blank samples were prepared with every na plant detectable levels. extraction batch. na water na (only mentioned in %) na water PFAS concentrations from 0.60 to 193 ng/L All results in article The method accuracy was assessed using the meansurrogate-corrected value from those same seven spikedreplicates and compared with the expected concentration. a 11-point calibration curve (from 0.05 to 500 g L-1 was generated , and thelinear correlation coefficient (r) was used for the qualification of linearity na na Method performance was evaluated through the recovery , linearity , precision and method detection and quantification limits studies Precision of the method (expressed in terms of relative standard deviation (RSD)) was evaluated from surface and wastewater samples spiked in triplicate at a concentration level of 1 g /L for each pollutant. Method detection limits (MDL) and method quantitation limits (MQL) were calculated in surface water Surface ranges from 0.010 to and in effluent wastewater as the water and 0.096 g /L concentrations of each compound effluent corresponding to a signal-to-noise ratio na water PFBuA: not detected of 3:1 and 10:1, respectively. facultative and aerated lagoons, chemically assisted (PFOA): 2.2 - 150 ng/L primary (influent) and 1.9 to 140 treatment, ng/L (effluent). secondary aerobic (PFOS): biological in primary sludge: 6.4 to treatment, 2900 ng/g dry weight (dw) and in waste advanced biological sludge, and biological treated biosolids: , 9.7 to nutrient 8200 ng/g dw, and 2.1 to removal 17,000 ng/g dw, na treatment respectively na Effluent from Municipal treatment plants: highest median concentrations of PFHxA (24 ng/L), followed by PFOA (23 ng/L), PFBA (19 ng/L), and PFOS (15 ng/L). PFPeA (9.7 ng/L), PFNA (9.0 ng/L), PFHxS (4.9 ng/L), and PFBS (2.8 ng/L). Low levels of the C6 and C8 PFPAs, PFHxPA (1.3 ng/L, median) and PFOPA (0.9 ng/L, median) were also na na detected. na 8:2 FTOH was the predominant congener, with concentrations of 2.10-11.0 ng/L, 3.05-12.4 ng/L, and 0.36- 1.91 ng/g dry weight in the influent, sludge and secondary effluent, and methods not been validated in na water sludge, respectively wastewater or sludge samples River water and WTTP na water na na Perfluorooctanoic acid (PFOA): in wastewater 1.3-28 ng/L and in sludge samples 117-673 pg/g Perfluorooctane sulfonate (PFOS): in wastewater: 0.9-9.8 ng /L and in sludge samples 98-683 domestic, pg/g hospotal The calibration and curves bracketed all quantified industrial *specific values pero concentrations in sample na WWTP PFAA are found in Table 3. extracts and displayed r2 values >0.99 na water 0.33 - 82.4 na na na up to 6231 ng/L. na na na na na sludge Samples were extracted in batches of 12 with each batch con-taining a method blank and a laboratory control sample ( Effluent from WWTP: 3.6106 to 1.3107 ng/L PFAS Wastewater drained from fire-fighting areas: 5.3 106 to 1.2 108 ng/L PFAS Runof water: 2.9 107 to 1.0 103 ng/L Lagoon: 2.3105 to na water 5.0105 ng/L na 9PFASs ranged from 0.98 - 440 ng/L (influent), 21 - waster and 560 ng/L (effluent) and na biosolids 5.2 - 150 ng/g (biosolids) na Concentrations were below the limit of na na quantification na PFAAs In tap water: up to 3890pg/L In influent: up to 6690 pg/ Analytical quality control included L procedural blank extractions, determination of compound-specific tap watter, in Effluent: up to method detection limits (MDLs), influent, 13000pg/L calculation of IS recoveries and precision effluent, testing na sludge in Sludge: up to 8820 pg/g through duplicate sample analysis. ranging from 0.05 to 1 ng/mL water Method accuracy ranged from 70 to127% for 49 of the 53 extracted PFAS, with the remaining four between 66 and 138%. Method precision ranged from 2 to 28%RSD, with 49 out of the 53 PFAS being below < 20%. Linear calibration curves were constructed for six to ninelevels by gravimetric dilution of 100 ng/mL native compoundmixture in MeOH drinking waters, ground waters , surface waters , influents, effluents ofnwastewa ter treatment plants up to 100 micro g /L leave-one-out cross-validation The mean of the sum concentration of the 22 other PFAS (PFAS22) in the biosolids samples ranged from 4.93 to 92.6 regression coefficients (r2) higher than na na ng/g d.w 0.99 were accepted. na na na na PFAS concentrations in effluent from Bugolobi wastewater treatment plant (WWTP) were higher (5.6-9.1 ng L-1) than in the corresponding in_x0002_fluent (3.4-5.1 ng L-1 ), indicating poor removal of PFASs within theWWTP.PFAS concentrations decreased by a factor of approximately five between Nakivubo channel (8.5-12 ng L-1 ) and Lake Victoria (1.0-2.5 ng L-1 ), due to dilution, sorption to sediment and uptake by plants in the wetland. PFAS concentrations were within the range 1700- 7900 pg g-1 dry weight (dw) in soil and 160 pg g-1 dw (maize cobs) to waster and 380 pg g-1 dw (sugarcane na sludge stems) in plants. na Waste water: PFOA in concentrations of 20- 73 ng/L PFOS up to 390 ng/L River water downstream: river PFOA: 11 +/-4 ng /L upstream, PFOS: up to 32 ng/L river downstrea river upstream: m, WWTP PFOA: 0-2 ng/L Calibration curves had regression na effluent PFOS: 0-1.5 ng/L coefficients of more than 0.995. na na na na main PFAS reported: inffluents: PFBA: 23.8 ng/L PFOA: 6.15 ng/L Effluents: PFBA: 20.2 ng/L PFOA: 6.07 ng/L sludge: PFOS: 2.13 ng/ g PFOA: 0.85 ng/ g other values found in Fig blank samples, LOD and LOQ were na na 2. defined. na na na na na na na na municipal WWTP effluents: sodium perfluoro-1- hexanesulfonate (4.7 ng/L), 8:2-FTS (1 ng/L), PFOA (3 ng/L), inffluent, and 6:2-FTS (4.7 ng/L). effluent, industrial industrial WWTP inffluent: and PFASs up to 700 g/L na municipal na na na na na Limitations LoD (ng/mL) subgroup Measurement - generic name Details in the Supplementary na Information na Total method detection na limits ranged between 0.1 and 0.5 ng/L na na 0.23 - 0.51 na future work is needed to identify FTCA precursors in landfills and to estimate the attenuation of FTCAs during wastewater treatment na na na na na na 0.02-0.45 na na Not in article na A large number of biosolids samples were combined to form five composites in this study in order to reduce the number of samples to be analyzed and still provide with a defensible mean baseline concentration for the analytes 0.03 and 0.14 ng/g dry weight (dw) of biosolids na IDL: PFBA -4.8, PFPeA - 0.15, PFHxA - 0.18, PFHpA - 0.10, PFOA - 0.66, PFNA - 0.30, PFDA - 0.17, PFUnA - 6.41, PFBS - 0.19, PFHxS - 0.18, PFOS - 0.80, and PFDS - 0.21 ; LOD stated as three times the na IDL na na na na na na Therefore, the limit of quantification (LOQ) was defined as the concentration in which sewage sludge samples yielded a reliable chromatographic peak. This was the case usually na for peaks with a signal intensity > 5E3. na Instrumental LOQs for F-53B and PFOS in this study were 0.14 and 0.15 ng/L, respectively, and instrumental LODs were 0.04 ng/L for na both na A challenge in very comprehensive screening methods are elevated blank values which have to be considered to avoid false positive findings. In this study this hindered the determination of the following ten compounds: the insect repellents diethyltoluamide (DEET) and icaridine, the plasticizers dibutyl adipate, N- butylbenzenesulfonam ide (NBBSA), triethyl phosphate (TEP), tris(2- butoxyethyl) phosphate (TBEP) and triphenyl phosphate (TPP), the UV filter octocrylene, the lubricant oleamide and the perfluorinated compound perfluorooctanoic acid (PFOA). mna na na na na na 0.2 ng/L na values ranged from 0.02 (6:2Cl- PFESA) ng/mL to 0.50 (PFBA) ng/mL. Many LOQ na values in the article na LOQ: 0.5 ng/L for water na samples and 0.1 g/kg d.w. for sludge samples na was determined as three na times the signal in the procedural blanks na na 0.12 - 0.75 na na na na LC-MS/MS Dilusion may reduce matrix effects na na LC-MS/MS na na na GC-MS na na na LC-MS/MS for each analyte na varied from 0.5 to 5.4 ng/ L na LC-MS/MS MDLs for each compound ranging from 0.030 to0.200 ng/g dry na weight na LC-MS/MS na na na LC-MS/MS The MDLs ranged between 0.06 na and 2 ng/L. na LC-MS/MS na na na LC-MS/MS na na na LC-MS/MS Minimum detection limit: 1.4 na ng/L na LC-MS/MS na na na LC-MS/MS na na na na na na LC-HRMS Surface water: 7.5 - 100 Seawater: 1-100 Sewage water: 5- na 100 na LC-HRMS na na na LC-MS/MS na LoQ: 10 g/kg na LC-MS/MS na na na LC-MS/MS na na na LC-HRMS na 0.1-1 na GC-MS na na na LC-MS/MS na na na LC-MS/MS na na Because of the low intensity and/or the limit fragments in MS/ MS spectra, there was no identified PFAS with a level 3 or above in ESI positive mode. Also, the extract of samples has been kept in -20 C for 6 years, and the identified PFASs could be the potential transformation products. na na LC-MS/MS na LC-HRMS ranging from 0.01- na 5; TFA: 34 na SFC-MS/MS, LC-MS/MS na na na TOPassay, LC-HRMS na na na LC-HRMS MQL varied from 0.19ng/L to na 0.49ng/L. na LC-MS/MS MDL (ng/L) = 0.7 (PFTriA) - 4.6 (PFBA, PFPeA), 47.2 (FDEA), 92.9 (FHEA), 106.8 (FOEA) na LC-MS/MS in ng/g Water: 0.03 - 1.08 for different coumpounds Fish: 0.0.1 - 0.0.9 Sediment: 0.01 - 2 Crab: 0.01 - 1.11 Plankton: 0.002 - 8.82 na Worms: 0.01 - 5.3 na LC-HRMS na na na LC-MS/MS na na na The method limits of detection were ranging in na general from 15 to 79 ng/kg. na LC-MS/MS na na na na na na GC-MS na na na LC-MS/MS na can be found in the Supplementary data na LC-HRMS na na na For four compounds, PFPS, PFNS, PFPeDA and PFHpA no standards were available. These compounds were quantified by parameters of the corresponding shorter and longer-chain PFCs The MQL ranged and are therefore only between 0.05 ng/L for estimations PFHxSi and 22.8 ng/L for PFDPA na LC-MS/MS na <0.2 ng g1 (dry sewage sludge) na LC-MS/MS na na na The ILOD for all of the targeted PFAS ranged between 0.01 and 0.25 ng mL1 , and the ILOQ values were in the range na of 0.05e0.7 ng mL1 na LC-MS/MS na 9.5 pg/g na LC-MS/MS na na na LC-HRMS na na na LC-MS/MS na na from 0.1 to 15 g/L recovery: 78% to 126 % na na LC-MS/MS na TOPassay na na na LC-HRMS na na na GC-MS na 0.2 - 0.4 na LC-MS/MS na na na GC-MS na na na GC-MS na not in report na LC-MS/MS na ~10 na LC-MS/MS The MDLs ranged from 0.28 to 18 ng/L and methodquantitation limits (MQLs) from 0.35 to 26 ng/L na (all details in article) na LC-MS/MS method quantification na limits < 1ng/L na LC-MS/MS (LOD) were 0.01 g L-1 for PFOA and PFOS; 0.50 g L-1 for NP, PrP, na PFBu, PFPeA, PFHpA; PFHxA, and na LC-MS/MS na na na LC-MS/MS na na na LC-MS/MS Influent: 0.05- 0.12 Secondary influent: 0.03-0.11 na Sludge: 0.01 - 0.07 na LC-MS/MS na MQL: 0.39-1.00 ng L-1 na LC-MS/MS limit of quanti_x0002_tation (LOQ) was 4 pg (absolute na amount) for the HPLCMS/MS method. na LC-MS/MS na 0.04-0.05 na LC-MS/MS na na LC-MS/MS na na na LC-MS/MS na na na LC-MS/MS na 4-25 na LC-MS/MS na na Concentrations were below the limit of quantification (three times the LDC) for perfluorinated acids na LC-MS/MS LC-HRMS PFBA and PFPeA: not result due to interferences. na na LC-MS/MS na not in paper na LC-MS/MS method detection limits na (0.014-0.44 ng/L) ) na LC-MS/MS na na na LC-MS/MS na na na LC-MS/MS water: 0.05 to 1.79 na solid: 20 to 2700 pg g-1 dry weight (dw) na LC-MS/MS The limits of quantification (LOQ, signal to noise ratio 7) for river and waste water were 0.06 and 0.12 ng/L PFOA and na 0.12 and 0.24 ng/L PFOS, respectively. na LC-MS/MS 0.6 (PFHxA), 0.3 (PFOA), 0.3 (PFDoDA), 0.8 na (PFHxS), and 0.2 ng/L (PFOS) na LC-MS/MS na provided in Tables S1-S3 na LC-MS/MS na 2.8 - 185.8 na LC-HRMS na 0.35 pg for PFOA pg for PFOS and 0.05 na LC-HRMS The inclusion of all analytes in only one HPLC-MS/MS experiment was impossible because of the different HPLC parameters needed, such as the flow rate and solvent composition of the injected samples. m 0.3 to 199 ng/L depending on the analyte and matrix na LC-MS/MS na na na LC-HRMS, LC-MS/MS Title A simple and sensitive gas chromatography-electron capture detection method for analyzing perfluorocarbon tracers in soil gas samples for storage of carbon dioxide Ultra trace detection of perfluorocarbon tracers in reservoir gases by adsorption/thermal desorption in combination with NICI-GC/MS Simultaneous determination of trace amounts of sulphur hexafluoride and cyclic perfluorocarbons in reservoir samples by gas chromatography Solid phase microextraction (SPME) sampling under turbulent conditions and for the simultaneous collecting of tracer gases Authors Nazzari et al. Galdiga et al. Galdiga et al. Susanne et al. Journal year International Journal of Greenhouse Gas Control 2013 Vol. 14 Pages 60-64 Fresenius Journal of Analytical Chemistry 2000 Vol. 367 Issue 1 Pages 43-50 Chromatographia 1997 Vol. 46 Issue 7-8 Pages 440-443 International Journal of Mining Science and Technology 2015 Vol. 25 Issue 4 Pages 559563 2013 2000 1997 2015 comments (t, nt, o) DOI link targeted 10.1016/j.ijggc.2012.12.029 targeted, see also construction products 10.1007/s002160051596 targeted targeted 10.1007/bf02490884 10.1016/j.ijmst.2015.05.007 Name perfluoromethylcyclohexane PMCH, perfluoro-1,2dimethylcyclohexane PDCH, perfluoromethylcyclopentane PMCP PMCP, PDMCB, PMCH, 1,2-PDMCH, 1,3-PDMCH perfluorodimethyl cyclobutane, perfluoromethyl cyclopentane, perfluoromethyl cyclohexane and the 1,2and 1,3isomers of perfluordimethyl cyclohexane SF6 and PMCH CAS (if available in source) na na na na Sampling sample amount used Samples are collected using a hollow steel probe driven into the ground to a depth of 0.6-0.8 m. through CarbotrapTM 100 graphitized carbon black na e tracer compounds were trapped in tubes filled with a carbon molecular sieve and in a two_x0002_step procedure thermally desorbed na pressurised gas from a North Sea reservoir na SPME under dynamic conditions na Pre- treatment na na na na Extraction na na na na Clean up na na na na Measurement thermal desorption autosampler, coupled to a gas chromatograph fitted with an electron capture detector (GC-ECD) adsorp_x0002_tion/thermal desorption in combination with NICI-GC/ MS All measurements were carried out with a NCI-ion source. The separations were carried out on an Al2O3 PLOT column (50 m 0.32 mm 0.8 m) GC-ECD, Carbopack C column and a 5A Molecular Sieve column GC-ECD Quantification method Working range (ng/mL) As external calibration procedure na na na na na na na Matrices Soil gas petroleum reservoirs gas na reported levels (ng/mL) na 42 femtoliter/liter na na info - validation of the method Limitations linear up to 500 pg, with R2 ranging between 0.989 and 0.993. within-day precision was between 5 and 11% between-day precision ranged from 6 to 15% na na na na na 1-2 % RSD na LoD (ng/mL) subgroup Measurement - generic name 1.3 to 5.8 fL/L na na na 10 EXP-15 [liter/liter] na ppb levels na GC-ECD GC-MS GC-ECD GC-ECD Title Authors Monitoring hydrofluorocarbon refrigerant leakage from air-conditioning systems in buildings Cheong et al. Determination of fluorochemical surfactants in acid etch baths by ion chromatography with online matrix elimination Laikhtman et al. Ultra trace detection of perfluorocarbon tracers in reservoir gases by adsorption/thermal desorption in combination with NICI-GC/MS Galdiga et al. Development and Validation of a Wipe Test Method Using Liquid Chromatography with Tandem Mass Spectrometry for the Determination of Perfluorooctanoate (PFO) on Various Surfaces Botelho et al. An optimized method for the determination of perfluorooctanoic acid, perfluorooctane sulfonate and other perfluorochemicals in different matrices using liquid chromatography/ion-trap mass spectrometry Dolman et al. Stability of Per- and Polyfluoroalkyl Substances in Solvents Relevant to Environmental and Toxicological Analysis Zhang et al. Structural isomers of polyfluorinated di- and trialkylated phosphate ester surfactants present in industrial blends and in microwave popcorn bags Trier et al. Determination of Perfluorooctane Sulfonates (PFOS) in Four Chemical Materials by HPLC/MS/MS Cheng et al. Previously unidentified sources of perfluoroalkyland polyfluoroalkyl substances from building materials and industrial fabrics Janousek et al. Screening for perfluoroalkyl acids in consumer products, building materials and wastes Becanova et al. Journal year Applied Energy 1996 Vol. 53 Issue 4 Pages 341347 Journal of Chromatography A 1998 Vol. 822 Issue 2 Pages 321-325 1996 1998 Fresenius Journal of Analytical Chemistry 2000 Vol. 367 Issue 1 Pages 43-50 2000 Journal of Occupational and Environmental Hygiene 2009 Vol. 6 Issue 7 Pages 390-395 2009 Journal of Chromatography B-Analytical Technologies in the Biomedical and Life Sciences 2011 Vol. 879 Issue 22 Pages 2043-2050 2011 Environ. Sci. Technol. 2021 Environmental Science and Pollution Research 2011 Vol. 18 Issue 8 Pages 1422-1432 2011 In: Advances in Chemistry Research Ii, Pts 1-3, edited by S. Chen, Z. T. Liu and Q. Z. Zeng 2012 Environmental Science Processes & Impact 2019 Chemosphere 2016 Comment DOI link bad - method is about emission rate of HFC's in buildings 10.1016/0306-2619(95)00027-5 bad - method is about surfactants 10.1016/s0021-9673(98)00631-1 bad - reservoir samples - no construction products 10.1007/s002160051596 bad - applicable only to nonporeus surfaces! Caution for the porous surfaces! 10.1080/15459620902911212 bad - only application of 1 sample (PTFE sealant) 10.1016/j.jchromb.2011.05.032 stability measurements 10.1021/acs.est.1c03979 bad - industrial bland is a standard mixture, only 1 sample is measured 10.1007/s11356-011-0488-2 bad - limited sample (only 1) 10.4028/www.scientific.net/AMR.554-556.1872 very good 10.1039/c9em00091g good https://doi.org/10.1016/j.chemosphere.2016.08.1 PFAS CAS (if available in publication) na na fluorochemical surfactant FC-93 na PMCP, PDMCB, PMCH, 1,2-PDMCH, 1,3-PDMCH na PFO na PFOA, PFOS na Twenty-one PFASs in four classes (i.e., 1 PFCA, 1 PFSA, 18 PFEAs, and 1 fluorotelomer sulfonate) na diPAPS . S-diPAPS . triPAPS na PFOS na peruoro carboxylicacids (C4-C14), peruoro sulfonic acids (C4-C8,C10and C12),n:2uorotelomer sulfonates (n: 2 FTS,n=4, 6 and 8),n:2FTOHs (n=6, 8 and 10), 2H,2H- peruorodecanoic acid (8 : 2FTCA), 2H,2H,3H,3Hperuoroundecanoic acid (8 : 3 FTCA),7H-peruoroheptanoic acid (7HPFHpA), peruoro-3,7-dimethyloctanoic acid (PF37DMOA) and peruorooctanesulfonamide (PFOSA). na peruoro carboxylicacids (C4-C14), peruoro sulfonic acids (C4-C8,C10and C12),n:2uorotelomer sulfonates (n: 2 FTS,n=4, 6 and 8),n:2FTOHs (n=6, 8 and 10), 2H,2H- peruorodecanoic acid (8 : 2FTCA), 2H,2H,3H,3Hperuoroundecanoic acid (8 : 3 FTCA),7H-peruoroheptanoic acid (7HPFHpA), peruoro-3,7-dimethyloctanoic acid (PF37DMOA) and peruorooctanesulfonamide (PFOSA). na Sampling sample amount used na na etch bath composed of HF-ammonium fluoride (1:6) and the fluorochemical surfactant FC-95 in an etch bath containing concentrated HF, HCl and HNO na e tracer compounds were trapped in tubes filled with a carbon molecular sieve and in a two_x0002_step procedure thermally desorbed na Wiping of surfaces na microwave popcorn bag brands A and B, non- stick baking paper brands A and B, a French fry box, sandwich wrapper, a hamburger box and PTFE sealant tape, one piece of 50 mg na PFAS standard solutions starting concentration of 50 g/L, Samples (100 L) A microwave popcorn bag extract 0.5 dm2 was taken from each of two bags na a total area of 50 cm2 was cut into small sections na 23 samples of building materials. 28 samples of industrial textiles. Mostly purchased directly but in some cases the manufacture's supplied the articles 1 gram 23 samples of building materials. 28 samples of industrial textiles. Mostly purchased directly but in some cases the manufacture's supplied the articles 1 gram Pre- treatment Extraction na na na na na na The wipe samples were extracted na off-line SPE na PFAS stability: The PFAS was subsequently dissolved in 10 mL of solvent [i.e., deionized water, methanol, acetonitrile (ACN), acetone, DMSO, or isopropyl alcohol (IPA)]. For experiments involving various water-to-organic solvent ratios, solvents of different compositions (100% organic solvent, 90:10% (v/v) or 80:20% (v/ v) organic solvent/water) were added. no extraction The strips were therefore fully Environ Sci Pollut Res (2011) 18:1422-1432 1423 immersed in 40 mL of 95% aqueous ethanol na accelerated solvent extraction (ASE) or solid phase extraction (SPE) na samples were cut and dried. Liquied-solid extraction was done with methanol and water. samples were cut and dried. Liquied-solid extraction was done with methanol and water. Clean up na na na na Measurement The concentration-decay technique was used to determine the air exchange rate in a room. The method is based on an initial injection of tracer gas to simulate refrigerant leakage, R134a was injected into the chamber with all the dampers closed and fans off. SF 6 was also released in the chamber in order to compare the accuracy of R 134a measurement of air exchange rates. A desk fan was used to assist the mixing of tracer gases and air in the chamber over a period of 10 min. Once a uniform concentration of tracer gases was achieved, dampers at the supply and extract ducts were opened and the fans were switched on. Monitoring of the concentrations of R 134a and SF 6 tracer gas then commenced simulta_x0002_neously at the centre of the chamber, using a multigas analyser, On-line matrix elimination 3 was accomplished on a polymeric reversed-phase column followed by separation on a multiphase HPLC column, and detection by suppressed conductivity adsorp_x0002_tion/thermal desorption in combination with NICI-GC/MS All measurements were carried out with a NCI-ion source. The separations were carried out on an Al2O3 PLOT column (50 m 0.32 mm 0.8 m) Column temperature: 30C Flow rate: 0.3 mL/min Injection volume: 5L Run time: 14 min Retention time: 6.7 min Mobile phase: Gradient Time (min) %A %B 0 90 10 5 10 90 9 10 90 10 90 10 14 90 10 A = 2mM ammonium acetate in water B = methanol reversed_x0002_phase liquid chromatography on a Phenyl-Hexyl column coupled with ion-trap (IT) mass spectrometric detection acetonitrile gradientin water from 20% to 50% in 6 min. As a cleaning step, the column was washed with 95% acetonitrile for 2 min and equilibrated for 7 min at 20% na acetonitrile Samples were taken at different times and diluted into 10 mL of deionized water in PP tubes and stored at room temperature until analysis. Measured at several temperatures. LC-MS analysis was performed using an Agilent 1290 Infinity II HPLC coupled to an Agilent 6545 quadrupole time-of-flight (QTOF) mass spectrometer. After 5 d, samples of degration products of HFPO-DA, HFPO-TA, and HFPO-TeA were taken and analyzed using a headspace gas chromatography-mass spectrometry (GC-MS) method. Waters Acquity BEH C18 column (1502.1 mm i.d., 1.7 m particle size) operated at 45C. The binary solvent system consisted of methanol/ distilled water 5:95 (v/v) (mobile phase A) and methanol (mobile phase B) A 35 min gradient elution programme was used with an initial composition of 95% A: 0-3 min linear to 40% A, 3-24 min linear to 5% A, 24-31 min linear to 2% A, 31-33 min curved to initial composition and isocratic from 33-35 min. The flow rate was 0.28 mL min-1 , and the column heater was at 45C The accurate mass measurements and MS2 analysis for structure elucidation were performed with a Micromass na quadrupole time-of-flight (QTOF) HPLC measurement was performed using Atlantis T3 C18 column with 2.1 mm 150 mm i.d. 5.0 m. The mobile phase was acetonitrile and 10 mmol/L ammonium acetate solution with a volume ratio of 4:1. The flow rate was 0.2 mL/min and the injection volume na was 10 L na HPLC-MS/MS na HPLC-MS/MS Quantification method Working range (ng/mL) As na na na na na na internal standard on a 10-cm 10-cm surface. The analytical method was evaluated over a range of 1 to 23 ng/cm2, When possible, quantification was conducted with an isotope dilution approach, in which the analyte response was normalized to that of an isotopically labeled analogue. For other PFASs, the analyte response was normalized to that of an isotopically labeled PFAS with an LC retention time similar to that of the analyte na na na na na Internal standard na Internal standard na Matrices Reported levels (ng/mL) info - validation of the metho Limitations emis_x0002_sion rate for R134a was found to be in the range 270.2- na 870.7 mg/h, na na 5 mg/l of the surfactant FC-93 in 100 ml of the the area R.S.D. was etch 0.6%, linear between 10 na bath and 50 mg/l na petroleum reservoirs 42 femtoliter/liter na six surfaces: stainless steel, polycarbonate, Formica, butyl acid suit material, laminated disposable suit material, and a painted surface na all recoveries are within acceptance limit criteria of 80% to 120% %RSD95 ranged from 1.9 to 6.6% na food packaging, polytetrafluoroethylene (PTFE) sealant tape and drinking water low ug/kg PFOA recover_x0002_ies between 75 and 78% and PFOS recoveries between 81 and 88 (RSD) of 1.9 and 2.8% na na na na na oil- and water-repellent coatings on paper and board na na na coatings of nonstick pot, food packaging materials, waterborne coatings containing fluoride and fire-fighting foams linear calibration curve was obtained in the range of 0.002 - 0.1 g/ mL recovery for PFOS was in the range of 93.4 - 103% with relative standard deviation of 0.48 - 3.59%. T na awning: 260 g/kg Seat Cover (car): 2-50 g/kg Coatings: 20-70 g/kg Foul (for facedes): 2-30 Blank samples were textiles, paint, foan, g/kg prepared with every glue, foil, coatings extraction batch. na awning: 260 g/kg Seat Cover (car): 2-50 g/kg Coatings: 20-70 g/kg Foul (for facedes): 2-30 Blank samples were textiles, paint, foan, g/kg prepared with every glue, foil, coatings extraction batch. na LoD (ng/mL) subgroup Measurement - generic name na na na na LC-MS/MS na na GC-MS 100 ng/wipe. na LC-MS/MS 25 pg/mL na LC-MS/MS na na LC-MS/MS na na LC-MS/MS 0.4 g/m2 na LC-MS/MS not in report na LC-MS/MS not in report na LC-MS/MS Title Occurrence and characteristics of perfluoroalkyl substances (PFASs) in electroplating industrial wastewater First Report of a Chinese PFOS Alternative Overlooked for 30 Years: Its Toxicity, Persistence, and Presence in the Environment Targeted and Nontargeted Analysis of PFAS in Fume Suppressant Products at Chrome Plating Facilities Multianalyte profiling of per- and polyfluoroalkyl substances (PFASs) in liquid commercial products Authors Journal year Jiawei et al. Wang et al. Water Sci Technol 2019 Vol. 79 Issue 4 Pages 731-740 2019 Environmental Science & Technology 2013 Michigan Department of Environment, Great Lakes, and Energy (EGLE) na Favreau et al. Chemosphere 2020 2017 comments (t, nt, o) DOI link na 10.2166/wst.2019.092 na 10.1021/es401525n na https://www.michigan.gov/document Also applied to AFFF 10.1016/j.chemosphere.2016.11.127 PFAS perfluorobutyric acid (PFBA), perfluorovalerate (PFPeA), perfluoroheptanoic acid (PFHpA), perfluoroproxic acid (PFOA), perfluoro NONYLIC acid (PFNA), perfluorodecanoic acid (PFDA), perfluoro twelve acid (PFDoDA) and perfluorooctyl sulfonic acid (PFOS), perfluorohexanic acid (PFHxA), perfluorohexanoic acid (PFUnDA), and perfluoro ten. Tri acid (PFTrDA), perfluoro butyl sulfonic acid (PFBS) and perfluorohexyl sulfonic acid (PFHxS), perfluorooctyl sulfonamide (FOSA), quantitative mixed standard PFACMXB, internal standard 13C4-PFOS, internal standard 13C4PFOA, internal standard 13C4-PFBA, and internal standard 13C2-PFDoDA chlorinated polyfluorinated ether sulfonate (locally called F53B, C8ClF16O4SK), PFOS Targeted analysis of 25 PFAS (4:2 FTS, 6:2 FTS, 8:2 FTS, GenX, N-EtFOSAA, N-MeFOSAA, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFOSA), non-targeted analysis 41 targeted PFAs including PFCAs (C4-C16), PFSAs (C4, C6, C8, C10), ipPFNS, PFPAs (C6, C8, C10), FOSA, N-Me FOSA, NEt FOSA, FASAAs: FOSAA, N-MeFOSAA, N-EtFOSAA, NMeFOSE, N-EtFOSE, FTSAs (4:2, 6:2, 8:2 FTS), FTOHs (4:2, 6:2, 7:2s, 8:2, 10:2), 8:2 FTI, 8:2 FTAC, 8:2 FTMAC CAS (if available in source) na na 757124-72-4 (4:2 FTS), 27619-97-2 (6:2 FTS), 39108- 34-4 (8:2 FTS), 13252-13-6 (GenX), 2991-50-6 (N- EtFOSAA), 2355-31-9 (N-MeFOSAA), 375-22-4 (PFBA), 2706-90-3 (PFPeA), 307-24-4 (PFHxA), 375-85-9 (PFHpA), 335-67-1 (PFOA), 375-95-1 (PFNA), 335-76-2 (PFDA), 2058-94-8 (PFUnDA), 307-55-1 (PFDoDA), 72629-94-8 (PFTrDA), 376-06-7 (PFTeDA), 375-73-5 (PFBS), 2706-91-4 (PFPeS), 355-46-4 (PFHxS), 375-92-8 (PFHpS), 1763-23-1 (PFOS), 68259-12-1 (PFNS), 335- 77-3 (PFDS), 754-91-6 (PFOSA) na Sampling water sampling surface water samples (5 L for each sampling point) were taken from the Oujiang River, at Wenzhou city, China the vicinity of where the discharge from a municipal WWTP enters the river. This WWTP is known to receive wastewater from the electroplating industry, where both F-53B and PFOS are assumed to be in use. Wastewater samples were also collected "upstream", at a small WWTP which treats the raw effluents of electroplating plants before they enter the municipal sewer system. 25 samples collected from fume suppressant products and effluents at 11 chrome plating facilities in Michigan Household products included impregnation agents (n = 60), cleansers (n = 24), polishes (n = 18), lubricants (n = 7). A miscellaneous category of products (n = 23) was defined by various applications that included foamsuppressing agents for the chromium industry, paints, ski wax, inks and tanning substances. sample amount used na 5 mL water samples (500 mL) 500 mg for LC-MS, 200 mg for GC-MS Pre- treatment Extraction purify by WAX columella na filtered through glass microfiber filters solid phase extraction (SPE) filtered extracted using a WAX solid phase, PFAS was removed from the cartridge in methanol extraction cartridge LC-MS: dissolved in 10 mL water, adding methanol/water, ammonium acetate (pH 4), GC-MS: dissolved in 10 mL methanol, filtration LC-MS: SPE with methanol/ ammonium acetate (50:50) Clean up Measurement LC-MSMS, Acclaim 120 C18 (4.6 150 mm, 5 m), mobile phase A was methanol, mobile phase B was 50 mM ammonium acetate solution, na the sample volume was 10 uL with 1 mL/min of flow rate extracts were reduced using a gentle stream of nitrogen, diluted to 1 mL with ultrapure water and filtered LC-MS/MS, ZORBAX Eclipse XDB C18 column (5 m 2.1 mm 150 mm, Agilent, CA) using an UltiMate 3000 HPLC (Dionex by Thermo Fisher Scientific Inc., MA), API 3200 triple quadrupole mass spectrometer (AB SCIEX, ON, Canada) UPLC-MS using targeted workflow methods described within volume reduced laboratory Quality Assurance Project Plan LC-MS: adding ammonium hydroxide in methanol (0.5 %), neutralized with acetic acid LC- MS/MS, GC-MS/MS for FTOHs, FTI, FTAC, FTMAC Quantification method Working range (ng/mL) As na na Potassium L-PFOS and 13C4- and 13C8-labeled L-PFOS, as recovery and injection standards na calibration curves derived from authentic standards, matched stable isotope labeled internal standard (when available) or a closely eluting labeled standard (when an exact match was not available) 10 to 150 ng/L internal standardisation using mass- labeled standards na Matrices reported levels (ng/mL) electroplating waste water drainage system: 229.5 to 5 410.6 ng/ L effluents is about 538 ng/L waste water (effluent and influent) 43-78 and 65-112 g/L for the effluent and influent, respectively fume suppressant sampling, effluent sampling The only PFAS compound observed in the fume suppressant products with targeted analysis was 6:2 FTS, which was present in very high concentrations in all products except product 3 where it was not detected household products (impregnation agents, cleanser, polishes), lubricants, 55% of all samples contained at least foamsuppressing agents for one PFAS between 0.1 and 25'000 the chromium industry, mg/kg of product, with the majority of paints, ski waxes, inks, products falling within the 100e1000 tanning substances, mg/kg range info - validation of the method Limitations LoD (ng/mL) recovery (90-127%) and reproducibility (1-15%) na average recovery was 100.1% with relative standard deviation of <10% na na Instrumental LOQs for F53B and PFOS in this study were 0.14 and 0.15 ng/L, respectively, and instrumental LODs were 0.04 ng/L for both relative percent difference (RPD), averaged 15% and no sample/analyte comparison exceeded the project goal of <30% RPD na LOQ 10 ng/L LOQ: 0.5-2 ng/mL (LC- na na MS), 2-10 ng/mL (GC-MS) subgroup Measurement - generic name na LC-MS/MS na LC-MS/MS na LC-MS/MS na LC-MS/MS, GC-MS Title Analysis of Perfluoro-carboxylic Acid Fluorides by Gas Chromatography/Mass Spectrometry Electrospray ionization time of flight mass spectrometry analysis of perfluoroalkyl acrylic oligomers synthesized using atom transfer radical polymerization Efficient "total" extraction of perfluorooctanoate from polytetrafluoroethylene fluoropolymer Adsorption of perfluorooctane sulfonate (PFOS) on mesoporous carbon nitride Adsorption of perfluorinated compounds on aminated rice husk prepared by atom transfer radical polymerization Distribution characteristics of trifluoroacetic acid in the environments surrounding fluorochemical production plants in Jinan, China Perfluoroalkyl acids (PFAAs) with isomer analysis in the commercial PFOS and PFOA products in China Characterizing direct emissions of perfluoroalkyl substances from ongoing fluoropolymer production sources: A spatial trend study of Xiaoqing River, China Occurrence and source apportionment of novel and legacy poly/perfluoroalkyl substances in Hai River basin in China using receptor models and isomeric fingerprints Isomer Profiles of Perfluoroalkyl Substances in Water and Soil Surrounding a Chinese Fluorochemical Manufacturing Park Authors Lou et al. Romack et al. Larsen et al. Yan et al. Deng et al. Xie et al. Journal year Chinese Journal of Analytical Chemistry 2013 Vol. 41 Issue 7 Pages 1086-1090 Abstracts of Papers of the American Chemical Society 2007 Vol. 233 2013 2007 Analyst 2006 Vol. 131 Issue 10 Pages 11051108 Rsc Advances 2013 Vol. 3 Issue 44 Pages 22480-22489 2006 2013 Chemosphere 2013 Vol. 91 Issue 2 Pages 124130 2013 Environ Sci Pollut Res Int 2020 Vol. 27 Issue 1 Pages 983-991 2020 Jiang et al. Chemosphere 2015 Vol. 127 Pages 180-187 2015 Shi et al. Li et al. Environmental Pollution 2015 Vol. 206 Pages 104-112 2015 Water Research 2020 Vol. 168 2020 Jin et al. Environmental Science & Technology 2015 Vol. 49 Issue 8 Pages 4946-4954 2015 comments (t, nt, o) DOI link no access na 10.3724/sp.J.1096.2013.21000 no link na 10.1039/b606801d na 10.1039/c3ra43312a na 10.1016/j.chemosphere.2012.11.015 na 10.1007/s11356-019-06689-4 na 10.1016/j.chemosphere.2015.01.049 na 10.1016/j.envpol.2015.06.035 na 10.1016/j.watres.2019.115145 na 10.1021/acs.est.5b00212 Name na na PFOA and APFO PFOS perfluorooctanoate (PFOA), perfluorobutanoic acid (PFBA) and perfluorooctane sulfonate (PFOS) TFA PFOS, PFOA per_x0002_fluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA), per_x0002_fluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), PFOA, PFNA, perfluorodecanoic acid (PFDA), perfuoroundecanoic acid (PFUnDA), perfluorododecanoic acid (PFDoDA), per_x0002_fluorotridecanoic acid (PFTrDA), perfluorotetradecanoic acid (PFTeDA), perfluorohexadecanoic acid (PFHxDA), per_x0002_fluorooctetradecanoic acid (PFODA), perfluorobutane sulfonic acid (PFBS), perfluorohexane sulfonic acid (PFHxS) and PFOS. In addi_x0002_tion, structural isomers of PFOA including LPFOA and four br_x0002_PFOAs (iso-, 5m-, 4m- and 3mPFOA) PFCAs (C4eC14), perfluoroalkyl sulfonic acids (PFSAs, C4eC10, even), PFOSA, Cl-PFESAs (6:2 and 8:2), FTS (4:2, 6:2 and 8:2), ammonium 4, 8-dioxa-3H-perfluorononanoate (ADONA), 6:2 diPAP, HFPO-DA, hexafluoropropylene oxide trimer acid (HFPO-TA), PFECHS na CAS (if available in source) na na na na na na na na na na Sampling na na na na aminated rice husk (RH) adsorbent sample amount used na na na na na Samples from flowing water bodies were collected from five sites air sampling was conducted at S1 using an annular glass denuder with a quartz fiber filter system d 1-kg soil samples from a depth of 0-10 cm were collected using undisturbed soil samplers All water samples were collected in pre-rinsed 500-mL polypropylene bottles na na na na na na sampling was conducted around a major fluorochemical manufacturing park in China in 2012, including soil and water collection inside the park, including from a wastewater treatment plant (WWTP), as well as in surrounding rivers and soil (15 km radius). na Pre- treatment na na pressurized solvent extraction (PSE) na Extraction na na na na na na After shaking, the filtrate was extracted by solid_x0002_phase extraction (SPE) using Oasis WAX SPE cartrid gas-phase sample, the two denuders were extracted with three consecutive additions of double-distilled water (10, 10, and then 5 mL) by transferring each addition from the first denuder to the second after shaking each denuder, and a com_x0002_bined extract (25 mL) was obtained. 10 g of each soil sample was placed into a 50-mL Erlenmeyer flask along with 30 mL of methanol na na na na na na na e extraction by Oasis WAX cartridges na Clean up na na na na na Measurement na na liquid chromatography with tandem mass spectrometry Kinetics studies reveal that the adsorption of perfluorooctane sulfonate (PFOS) HPLC with conductivity detector HPLC with a conductivity detector The method for detecting TFA was developed by Taniyasu na et al. (2008) PFAAs and the isomers of PFOS and PFOA were analyzed on high performance liquid chromatography couple with tandem mass spectrometry (HPLC-MS/MS) using the method developed by Benskin et al. (2007) FluoroSep RP Octyl column (ES Industries, West Berlin, NJ) at 38 _x0003_C. The mobile phase started from 60% A (HPLC grade water adjusted to pH 4.0 with ammonium formate) and 40% B (methanol) at a flow rate of 150 lL min_x0003_1 . The initial condition was held for 0.3 min and then ramped to 64% B by 1.9 min; increased to 66% B by 5.9 min, 70% B by 7.9 min, 74% B by 26 min, 80% B by na 30 min, and finally to 100% B by 37 min All samples were treated according to previously developed na methods (Zhou et al., 2013) na LC-MSMS high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) also paired with na an ultrahigh resolution orbitrap mass spectrometer Quantification method na na external calibration na na Working range (ng/mL) As na na na na na Matrices na na Polytetrafluoroe thylene fluoropolymer resin na na PFOS isomers (n-, iso-, 5m-, 4m-, 3m-, 1m-, m2-) and those of PFOA (n-, iso-, 5m-, 4m- and 3m-) were quantified using a characterized technical standard and isomer- specific product ions Riverine discharges of PFOA (23e67 t/ yr) were in agreement with theoretical emission calculations from FP production (68 t/yr) na water na na na na na water and sediment na na na na reported levels (ng/mL) na na adsorption capacities of MCN-1 calcined at 673, 773 and 873 K are 625.0, 555.5 and 433.7 mg g_x0001_1 adsorption capacities of PFOA, PFBA and PFOS on the aminated RH at pH 5.0 were 2.49, 1.70 and 2.65 mmol g_x0002_1 , 250-3000 ng/L water <0,1-2,6 ng/g in soil 1000-7000 pg/m3 air The purity of the three PFOS products was 76.7-80.6%. The major impurity in the PFOS products is PFOA, which contributes more than 10%. Other impurities include perfluorohexane_x0002_sulfonate (PFHxS), perfluorohexanoate (PFHxA) and perfluoroheptanoate acids (PFHpA). The percentage of linear PFOS (n-PFOS) in the three products was 66.2-71.9%, similar to that in the product manufactured by 3M (70.3%). The purity of the five PFOA products was relatively high (94.0-95.8%), and the major impurity was PFOS (2.06-3.09%). The percentage of n-PFOA in the five PFOA products was 76.4-77.9%, which was similar to that in the 3M PFOA (78%) Substantially elevated PPFAS concentrations downstream of tributary 4 demonstrated that the emissions from this FP manufacturer dominated total riverine discharges. Isomer profiles of per_x0002_fluorooctanoic acid (PFOA) in water displayed a stepwise increase in percentage branched PFOA down_x0002_stream of tributary 3 (14.0%) and 4 (22.7%) reflecting the importance of FP sources PPFAS concentrations ranging from 36.5 to 496 000 ng/L. PPFASs in sediment ranged from 0.333 to 4100 mg/kg dw and PFOA was the main homologue (18.1e95% of PPFASs). The total concentrations of PFASs (PPFASs) ranged from 1.74 to 172 ng/L, with perfluorooctanonate (PFOA) as the dominant compound (15.2% Unmix, was introduced to identify the sources of PFASs in the surface water, and the results indicated that fire-fighting foam/fluoropolymer processing aids (36.6%) trace the manufacturing sources of PFOA. Electrochemical fluo_x0002_rination (ECF) was the major PFOA manufacturing source with considerable contribution by telomeri_x0002_zation. Perfluoroalkyl sulfonates (PFSAs) were lower than perfluoroalkyl carboxylates (PFCAs) in all samples, and short-chain (C4-C6) PFCAs were predominant. Perfluoroalkyl phosphonates and phosphate diesters were occasionally detected, but at low detection frequency. Branched isomers of perfluorobutanesulfonate (PFBS) are reported for the first time, accounting for 15-27% of total PFBS in water. An enrichment of isopropyl_x0002_PFOA (28%) was found in WWTP influent, suggesting its manufacturing primarily by isopropyl telomerization. PFOA was still a major chemical in use at this site, primarily from isopropyl telomerization. info - validation of the method na na Limitations na na acceptable recovery range of 70 to 130% na na na instrument blank, solvent blank, and sam_x0002_pling site blank The detection limit and the limit of quantitation were calculated as 3 and 10 times the signal-to-noise ratio (S/N), respectively. The recoveries for the soil samples ranged from 91.3 to 95.8%. The recoveries for the water samples ranged from 93.1 to 94.8%, and the RSDs ranged from 2.1 to 6.2%. The recoveries of the atmospheric samples ranged from 91.4 to 93.7%, and the RSDs ranged from 1.5 to 2.1%. na LoD (ng/mL) na na 0.5 ppb, na na na na na na recoveries ranged from 70.4 8.7% to 109.2 4.1% in water and from 81.5 2.1% to 103.3 4.0% in sediment na na The recoveries of all the target PFASs were in the range of 65.7e129%, 73.5e119% and 59.8e137% na na The recoveries of all target compounds were in the range of 47-124% and 52-109% na na subgroup na na na na na Measurement - generic name LC-MS/MS LC-ECD na na LC-MS/MS na na LC-MS/MS na LC-MS/MS Title Elucidation of contamination sources for poly- and perfluoroalkyl substances (PFASs) on Svalbard (Norwegian Arctic) Simultaneous measurement of ventilation using tracer gas techniques and VOC concentrations in homes, garages and vehicles A pilot study of per- and polyfluoroalkyl substances in automotive lubricant oils from the United States Side-chain fluorotelomer-based polymers in children car seats Authors Skaar et al. Batterman et al. H. K. Zhu and K. Kannan Journal year Environ Sci Pollut Res Int 2019 Vol. 26 Issue 8 Pages 7356-7363 2019 Journal of Environmental Monitoring 2006 Vol. 8 Issue 2 Pages 249-256 Environmental Technology & Innovation 2020 Vol. 19 Pages 8 2006 2020 Wu et al. Environmental Pollution 268 (2021) 115477 2021 comments (t, nt, o) DOI link targeted 10.1007/s11356-018-2162-4 targeted 10.1039/b514899e 10.1016/j.eti.2020.100943 PIGE, XPS, LC-MS, GC-MS, TOPassay https://www.sciencedirect.com/scienc PFAS C4-C13 PFCAs (i.e. PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTriDA); C4, C6, and C8 PFSAs (i.e. PFBS, PFHxS, PFOS) and 6:2 fluorotelomer sulfonate (6:2 FTSA) hexafluorobenzene [392-56-3], octa_x0002_fluorotoluene [434-64-0], perfluoro (1,2-dimethylcyclobutane) [28677-00-1], perfluoro(methylcyclohexane) [355-02-2], and perfluoro(methylcyclopentane) [1805-22-7]. na PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFHxDA, PFPrS, PFBS, PFPeS, PFHpS, PFOS, PFNS, PFDS, Cl-PFOS, 4:2-FTSA, 8:2-FTSA, 8:2FTCA, FOSA, MeFOSA, EtFOSA, 6:2-FTOH, 8:2-FTOH, 8:2FTOH, 10:2-FTOH, EtFOSE, 6:2-FTAc, 8:2-FTAc, 10:2-FTAc, 6:2-FTMAc,, 8:2-FTMAc CAS (if available in source) na [392-56-3], [434-64-0], [28677-00-1], [355-02-2], and [1805-22-7]. na na Sampling sample amount used Soil, freshwater (lake, draining rivers), seawater, meltwater run-off, surface snow and coastal sediment 2.5 g of soil and 1000-2300 mL of aqueous samples active or passive samplers na na na Eighteen children's car seats, representing twelve brands, were purchased new by the Ecology Center as part of a project analyzing chemical additives in car seats Samples were cut into small pieces using scissors pre-cleaned with dichloromethane and methanol Pre- treatment water samples (Jahnke et al. 2007; Mller et al. 2010) and soil samples (Powley et al. 2005) na na No additional treatment was performed for samples prepared for PIGE and XPS analyses. Extraction na na Briefly, 50-100 mg of material was spiked with 20 ng each of the surrogate standards, and extracted with 4:1 hexane/isopropanol twice followed by 1:1 methanol/acetonitrile. For each extraction step, the sample was sonicated for 30 min and then centrifuged at 3000 rpm for 5 min. The supernatants were combined, reduced in volume to ~5 mL. Clean up na na cleaned-up with ~100 mg Envi-Carb graphite by vortexing for 1 min and centrifuging for 5 min. Measurement validated quantification methods for the trace analytical determination of PFASs GC-MS Quantification method na na article-included gamma ray emission spectroscopy (PIGE), Xray photoelectron spectroscopy (XPS), as well liquid and gas chromatography mass spectrometry (LC/MS and GC/MS) and TOP assay na Working range (ng/mL) As na na Matrices water reported levels (ng/mL) m 0.4 to 4 ng/L in surface lake water FFTS meltwater run-off (118 ng/L) run-off water (113-119 ng/L) and soil (211-800 ng/g) gas na FAS were detected in 97% of the car seat samples analyzed with MS, with total concentrations of 43 PFAS na car seats (PPFAS) up to 268 ng/g info - validation of the method Limitations LoD (ng/mL) detection limits (LOD), quantifica_x0002_tion limits (LOQ) and recoveries na na na na na The recoveries of surrogate standards were generally in the range of 60 -130% with some exceptions. Matrix spike recoveries of each individual compound were all within the range 75-125% for all the treatments. na PIGE measures total fluorine (organic and inorganic) with a sensitivity at the mg/g levels while XPS can distinguish organic and inorganic fluorine was only reliable for samples with fluorine content greater than 500 - 1000 mg/g. subgroup Measurement - generic name na LC-MS/MS na GC-MS PIGE, XPS, LC-MS/MS, GC- na MS, TOP assay Title Authors Journal Perfluorinated compounds and total and extractable organic fluorine in human blood samples from China Yeung et al. Environmental Science and Technology 42(21): 8140-8145 Combustion ion chromatography for extractable organofluorine analysis Aro et al. iScience, 24(9) Enantioseparation of chiral perfluorooctane sulfonate (PFOS) by supercritical fluid chromatography (SFC): Effects of the chromatographic conditions and separation mechanism Zhao et al. Chirality 2019 Vol. 31 Issue 10 Pages 870-878 Selective extraction of perfluorooctane sulfonate in real samples by superparamagnetic nanospheres coated with a polydopamine-based molecularly imprinted polymer Lin et al. J Sep Sci 2021 Vol. 44 Issue 5 Pages 1015-1025 Enantiomer Fractions of Chiral Perfluorooctanesulfonate (PFOS) in Human Sera Wang et al. Environ. Sci. Technol. 2011, 45, 8907-8914 Are humans exposed to increasing amounts of unidentified organofluorine Yeung et al. Environ. Chem. 2016, 13, 102- 110 Assessing exposure to legacy and emerging per- and polyfluoroalkyl substances via hair - The first nationwide survey in India Ruan et al. Chemosphere 2019 Vol. 229 Pages 366-373 Exposure assessment to parabens, bisphenol A and perfluoroalkyl compounds in children, women and men by hair analysis Martin et al. Hand Wipes: A Useful Tool for Assessing Human Exposure to Poly- and Perfluoroalkyl Substances (PFASs) through Hand-to-Mouth and Dermal Contacts Poothong et al. Science of the Total Environment 2019 Vol. 695 Environ Sci Technol 2019 Vol. 53 Issue 4 Pages 1985-1993 Screening of Poly- and Perfluoroalkyl Substances (PFASs) and Extractable Organic Fluorine (EOF) in the Blood of Highly Exposed People Aro et al. na Determination of 21 perfluoroalkyl substances and organophosphorus compounds in breast milk by liquid chromatography coupled to orbitrap high-resolution mass spectrometry Beser et al. Anal Chim Acta 2019 Vol. 1049 Pages 123-132 Perfluorinated substances in the Flemish population (Belgium): Levels and determinants of variability in exposure Colles et al. Chemosphere 2020 Vol. 242 Levels of Perfuoroalkyl Acids (PFAAs) in Human Serum, Hair and Nails in Guangdong Province, China: Implications for Exploring the Ideal BioIndicator Liu et al. Archives of Environmental Contamination and Toxicology A liquid chromatography-high resolution mass spectrometry method for the determination of thirty-three per- and polyfluoroalkyl substances in animal liver Barola et al. Journal of Chromatography A 2020 Vol. 1628 Pages 11 Comparison of extraction methods for per- and polyfluoroalkyl substances (PFAS) in human serum and placenta samples-insights into extractable organic fluorine (EOF) Kaiser et al. Analytical and Bioanalytical Chemistry 2021 Vol. 413 Issue 3 Pages 865-876 Determination of perfluoroalkyl substances (PFAS) in human hair by liquid chromatography-high accurate mass spectrometry (LC- QTOF) Piva et al. Journal of Chromatography B- Analytical Technologies in the Biomedical and Life Sciences 2021 Vol. 1172 Extractable Organofluorine Analysis in Pooled Human Serum and Placental Tissue Samples from an Austrian Subpopulation --A Mass Balance Analysis Approach Kaiser et al. Environ. Sci. Technol. 2021, 55, 13, 9033-9042 A Comparative Analysis of Perand Polyfluoroalkyl Substances (PFAS) and Extractable Organofluorine (EOF) Using Solid Phase Extraction-Weak Anion Exchange and Ion Pair Extraction in Serum Marichal Salameh Bachelor thesis Extractable organofluorine analysis: A way to screen for elevated per- and polyfluoroalkyl substance contamination in humans? Aro et al. Environment International Per- and Polyfluoroalkyl Substances (PFAS) in Facemasks: Potential Source of Human Exposure to PFAS with Implications for Disposal to Landfills Muensterman et al. Environ. Sci. Technol. Lett. 2022, 9, 320-326 Biomarkers, matrices and analytical methods targeting human exposure to chemicals selected for a European human biomonitoring initiative. Vorkamp et al Environment International, 2021, 146, 106082. PFASs: What can we learn from the European Human Biomonitoring Initiative HBM4EU. Uhl M, Schoeters G, Govarts E, Bi Int J Hyg Environ Health. year Comments DOI link 2008 na 10.1021/es800631n 2021 na 10.1016/j.isci.2021.102968 2019 targeted 10.1002/chir.23120 2021 targeted 10.1002/jssc.202000824 2011 na 10.1021/es2023434 2016 na 10.1071/EN15041 2019 na 10.1016/ j.chemosphere.2019.04.195 2019 na 2019 targetted 10.1016/j.scitotenv.2019.133864 10.1021/acs.est.8b05303 2019 na na 2019 na 10.1016/j.aca.2018.10.033 2020 na 10.1016/ j.chemosphere.2019.125250 2020 na 10.1007/s00244-020-00743-w 2020 na 10.1016/j.chroma.2020.461442 2021 na 10.1007/s00216-020-03041-5 2021 na 10.1016/j.jchromb.2021.122651 2021 na 10.1021/acs.est.1c00883 2021 na na Suggested workflow for rapid screening of samples for elevated PFAS contamination is proposed (based on Koch et al. 2022 2020) https://www.sciencedirect.com/sc 2022 These preliminary findings indicate that wearing masks treated with high levels of PFAS for extended periods of time can be a notable source of exposure and have the potential to pose a health risk. 3 new PFAS were found with the suspect screening https://pubs.acs.org/doi/10.1021/ Recommended standard method for target analyses of PFAS in 2021 human samples 10.1016/j.envint.2020.106082 2023 10.1016/j.ijheh.2023.114168. PFAS CAS (if available in publication) PFOS, PFHxS, PFOSA, PFDoDA, PFUnDA, PFDA, PFNA, PFOA, PFHpA, and PFHxA na Fluoride standard solution Anion multi-element standard Perfluorooctanoic acid Perfluoro-n-butanoic acid Perfluoro-n-[1,2-13C2]octanoic acid Perfluoro-n-[1,2-13C2]undecanoic acid Potassium perfluoro-1-butanesulfonate Sodium perfluoro-1-[13C8]-octanesulfonate Sodium perfluoro-1-dodecanesulfonate Sodium 1H,1H,2H,2H-perfluorooctane sulfonate (6:2) N-methylperfluoro-1-octanesulfonamide 2-Perfluorooctyl ethanol (8:2) Sodium bis(1H,1H,2H,2H_x0002_perfluorodecyl)phosphat e Perfluorooctylphosphonic acid Potassium 9-chlorohexadecafluoro-3-oxanonane- 1-sulfonate 2,3,3,3-Tetrafluoro-2-(1,1,2,2,3,3,3- heptafluoropropoxy)propanoic acid na perfluoro-1-methylheptane sulfonate (1 m-PFOS) 1 m-, 3 m-, 4 m-, 5 m-, and 4,5m2-PFOS na PFOS na racemic -1m PFOS na PFCAs (C5-C14), PFSAs (C4-C8, C10), FOSAs (H, Me, Et), FOSAAs (H, Me, Et), di-SAmPAP, FTCAs (3 : 3, 5 : 3, 7 : 3), FTUCAs (6 : 2, 8 : 2, 10 : 2), monoPAPs (6 : 2, 8 : 2), diPAPs (4 : 2, 4 : 2/6 : 2, 6 : 2, 6 : 2/8 : 2, 8 : 2, 8 : 2/10 : 2, 10 : 2), PFPAs (C6, C8, C10), PFPiAs (C6/C6, C6/C8, C6/C10, C6/C12, C8/C8, C8/C10, C8/C12), FTSAs (4 : 2, 6 : 2, 8 : 2) and FTSASs (6 : 2, 8 : 2) na na na perfluorobutanoic acid (PFBuA), perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), PFOA, PFOS na na na na na na na perfluorohexane sulfonic acid (PFHxS), PFOA, perfluorononanoic acid (PFNA) and perfluorobutane sulfonate (PFBS) na na na na na perfluorocarboxylic acids (PFCAs: C4-C14), perfluo rosulfonic acids (PFSAs: C4-C10), perfluorooctane sulfon_x0002_amides (perfluoro-n-octane sulfonamide (FOSA), N-ethyl_x0002_perfluoro-n- octane sulfonamide (EtFOSA)), N- ethyl_x0002_perfluoro-n-octane sulfonamido acetic acid (EtFOSAA), N-ethyl-perfluoro-n-octane sulfonamido ethanol (EtFOSE), fluorotelomer sulfonates (FTSAs: 4:2, 6:2, and 8:2), polyfluoroalkyl phosphate diesters (diPAPs: 6:2/6:2, 6:2/8:2, 8:2/8:2), polyfluorinated ether acids (ADONA and GenX), and 6:2 Cl-PFESA (F-53B)) na 11-chloroeicosafluoro-3-oxaunde_x0002_cane-1- sulfonic acid (11Cl-PF3OUdS); 9- chlorohexadecafluoro-3-oxano_x0002_nane-1- sulfonic acid (9Cl-PF3ONS); Perfluoro-n-butanoic acid (PFBA); perfluoro-1-butanesulfonic acid (PFBS); Perfluoro- n-decanoic acid (PFDA); Perfluoro-n-dodecanoic acid (PFDoA); perfluoro(2- ethoxyethane)sulfonic acid (PFEESA); perfluoro-1- heptanesulfonic acid (PFHpS); Perfluoro-n-heptanoic acid (PFHpA); perfluoro-1- hexanesulfonic acid (PFHxS); Perfluoro-n-hexanoic acid (PFHxA); perfluoro-3-methoxypropanoic acid (PFMPA); perfluoro-4- methoxybutanoic acid (PFMBA); Perfluoro-n- nonanoic acid (PFNA); perfluoro-1-octanesulfonic acid (PFOS); Perfluoro- n-octanoic acid (PFOA); Perfluoro-n-pentanoic acid (PFPeA); perfluoro-1- pentanesulfonic acid (PFPeS); perfluoroundecanoic acid (PFUnA); dodecafluoro-3H-4,8-dioxanonanoic acid (ADONA) na na PFCAs (C4 - C12), PFSAs (C4, C6, C8) and 6:2 FTSA na 63 different PFAS; TFA, PFPrA, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTDA, PFHxDA, PFOcDA, PFEtS, PFPrS, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFDoDS, 3:3 FTCA, 5:3 FTCA, 6:2 FTUCA, 7:3 FTCA, 8:2 FTUCA, 10:2 FTUCA, FBSA, MeFBSA, PFHxSA, MeFHxSA, FOSA, FOSAA, MeFOSAA, EtFOSAA, 4:2 FTSA, 6:2 FTSA, 8:2 FTSA, 10:2 FTSA, 6:2 Cl-PFESA, 8:2 Cl-PFESA, PFECHS, 6:2 mPAP, 8:2 mPAP, 10:2 mPAP, 6:2 diPAP, 6:2/8:2 diPAP, 8:2 diPAP, 10:2 diPAP, SAmPAP, diSAmPAP, PFHxPA, PFOPA, PFDPA, C6/C6 PFPiA C6/C8 PFPiA, C8/C8 PFPiA, HFPO-DA (GenX), ADONA na nonvolatile PFAS: PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA, PFTeDA, PFHxDA, PFPrS, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFDoS, Cl-PFOS, PFEtCHxS, FBSA, FHxSA, FOSA, MeFOSA, EtFOSA, FOSAA, MeFOSAA, EtFOSAA, 4:2-FTS, 6:2-FTS, 8:2- FTS, 10:2-FTS, 6:2-FTCA, 8:2-FTCA, 10:2-FTCA, 3:3- FTCA, 5:3-FTCA, 7:3-FTCA, 6:2-UFTCA, 8:2-UFTCA, ADONA, 9Cl-PF3ONS, 11-PF3OUdS, HFPO-DA, 6:2- diPAP, 8:2-diPAP, diSAmPAP volatile PFAS: 4:2-FTOH, 6:2-FTOH, 8:2-FTOH, 10:2-FTOH, 12:2-FTOH, MeFOSA, EtFOSA, MeFOSE, EtFOSE, 4:2-FTAc, 6:2-FTAc, 8:2-FTAc, 10:2-FTAc, 6:2-FTMAc, 8:2-FTMAc suspect volatile PFAS: 14:2-FTOH, MeFPrSE, MeFBSE, MeFPeSE, MeFHxSE, MeFHpSE, EtFEtSE, EtFPrSE, EtFBSE, EtFPeSE, EtFHxSE, EtFHpSE, 4:2- FTI, 6:2-FTI, 8:2-FTI, 10:2-FTI, PFBI, PFHxO, PFOI, PFDI, 6:2-FTO, 8:2-FTO, 10:2-FTO, 12:2-FTO na nonvolatile PFAS: PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA, PFTeDA, PFHxDA, PFPrS, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFDoS, Cl-PFOS, PFEtCHxS, FBSA, FHxSA, FOSA, MeFOSA, EtFOSA, FOSAA, MeFOSAA, EtFOSAA, 4:2-FTS, 6:2-FTS, 8:2FTS, 10:2-FTS, 6:2-FTCA, 8:2-FTCA, 10:2-FTCA, 3:3FTCA, 5:3-FTCA, 7:3-FTCA, 6:2-UFTCA, 8:2-UFTCA, ADONA, HFPO-DA, 6:2-diPAP, 8:2-diPAP, diSAmPAP nonvolatile PFAS: PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA, PFTeDA, PFHxDA, PFPrS, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFDoS, Cl-PFOS, PFEtCHxS, FBSA, FHxSA, FOSA, MeFOSA, EtFOSA, FOSAA, MeFOSAA, EtFOSAA, 4:2-FTS, 6:2-FTS, 8:2FTS, 10:2-FTS, 6:2-FTCA, 8:2-FTCA, 10:2-FTCA, 3:3FTCA, 5:3-FTCA, 7:3-FTCA, 6:2-UFTCA, 8:2-UFTCA, ADONA, HFPO-DA, 6:2-diPAP, 8:2-diPAP, diSAmPAP Sampling na sample amount used na na na na na na na Pregnant Women, "High-Exposure" Family na na na A total of 39 samples were collected from 14 different 73 cities of 11 states na Hair samples were collected from 42 volunteers Hair samples were washed first with ultrapure water, then with SDS (0.1%, w/v), and finally twice again with ultrapure water na n hand wipe samples collected as a composite sample from 23 both hands of 60 adults na na na They were collected by mothers, in different stages after birth, in a glass container using a breast pump na na na human serum (n=60), hair (n=49) and nails (n=39) na wild boar liver samples Aliquots of 30 g mashed liver The solid-phase extraction of serum using hydrophilic-lipophilic bal_x0002_ance sorbent (SPE-HLB) was adapted from the work of Kuklenyik and co-workers The preparation of placental tissue was adapted based on the method developed by Martin and co-workers na All hair samples for analysis were collected from the vertex posterior region na 36 human maternal blood, 136 placental tissue, and 136 cord blood samples For the serum pool samples, 600 L from two to four individuals were pooled. For placental tissue pools, individual samples were pooled using 1.5-3 g per sample na na We obtained 20 whole blood samples (1-2 mL) from 20 randomly selected participants in a longitudinal study with a wide range of PFAS levels due to longstanding exposure to drinking water contaminated by AFFF firefighting foams. Additionally, 9 randomly selected samples from a nearby municipality with uncontaminated drinking water was obtained, thus representing background PFAS exposure. 0.5 - 1.6 mL blood Facemasks were purchased from local stores in Notre Dame, IN 0,1-1 ml blood, plasma or serum 0,1-1 ml blood, plasma or serum Pre- treatment Extraction improved extraction (ion pairing) and cleanup (ENVI-carb and solid phase extraction) na extraction and SPE-WAX na na na Extraction experiments for the spiked samples with different PFOS concentrations (5-200 ng/L-1 ) were con_x0002_ducted under the optimized conditions. Briefly, 100 mL of water sample or 50 mL pretreated human serum sample was added into a polypropylene flask (pH = 3), 100 mg of MIPDA@Fe3O4 was added to the solution, and the mixture was sonicated for 2 min. Then the solution was transferred to a thermostatic bath and agitated at 150 rpm (298 K) for 30 min, to facilitate mass transfer and adsorption of the PFOS onto MIPDA@Fe3O4. The MIPDA@Fe3O4 was isolated using an external magnetic field and the supernatant was discarded. Then the col_x0002_lected magnetic adsorbents were transferred to a 50 mL polypropylene flask, with 10 mL methanol added as a des_x0002_orption solvent. The mixture was shaken in a thermostatic bath (150 rpm, 298 K) for 10 min and the eluent was then dried under a gentle nitrogen na na na modified ion-pair extraction method at pH 4 and pH 10 na hair samples were washed stepwise Extraction method was adopted after reviewing the previous methods based on organic solvent extraction followed by clean up (Li et al., 2013; Kim and Oh, 2017; Alves et al., 2015) extract were applied to Envi-Carb cartridge (100 mg, 1 mL, 100-400 mesh, Supelco, USA) for cleanup to achieve quick analysis na Target compounds were extracted and analysed by a previously re_x0002_ported method (Martn et al., 2016). na sonicated na na na extraction and clean-uThe analytical method described below has been developed and modified on the basis of a previous study for PFAS analysis carried out by Lankova et al. procedure based on the QuEChERs methodology f na na na The serum samples without any pre-treatment were used to analyze TF. The separate pretreatment of extracting EOF and PFAAs from serum samples, which was described in detail by Yeung et al. (2013), The pre-treatment of extracting PFAAs and EOF from nails and hair samples was depicted by Wang et al. (2018). na extracting liver with acetonitrile followed by two clean-up steps The extraction and purification protocol was performed according to Krrman et al. na n (ion-pair liquid-liquid extraction, solid-phase extraction (SPE), using hydrophilic_x0002_lipophilic (HLB) or weak anion exchange (WAX) sorbents) na 100 mg of hair were weighted in a polypropylene vial and 10 l of mass labelled I.S. were added. Two ml of acetonitrile were added up carefully to soak all the material before extraction in ultrasound bath at 45 C for 45 min. The extract was collected in a separated polypropylene vial and the extrac_x0002_tion procedure was repeated another time. Finally, extracts were collected in the same vial (4 ml total volume). Sample clean-up was by solid phase extraction (SPE) by using Bond elut-ENV cartridges. na The serum samples were prepared using solid phase extraction with a weak anion exchange sorbent (SPE-WAX), modified from Kuklenyik et al. (2004) The placental tissue samples were extracted with a method adapted from Martn et al. (2016) (16) with an EnviCarb clean-up step 61 investigated PFAS, sample preparation, and the extraction procedure are shown in the study by Kaiser et al. (2020) na ion-pair extraction (IPE) and solid phase na extraction with weak anion exchange (SPE-WAX). First, 2 mL of 0.5 M TBA solution in water and 5 mL of MTBE were added to the sample (0.5-0.7 mL of blood for Replicate 1 and 0.5-1.6 mL for Replicate 2). Then the mixture was shaken horizontally at 250 rpm for 15 min and after that centrifuged for 10 min at 8500 rpm (8000 g). The extraction was repeated twice with 3 mL of MTBE, after collecting the organic solvent layer. The organic solvent extracts from all three cycles were combined and evaporated to 0.2 mL under a stream of nitrogen, then reconstituted to 1.0 mL with MeOH and evaporated to a final volume of 0.5 mL. TF-analysis: Facemasks were cut to 2 2 cm2 pieces with methanol rinsed scissors and were mounted to a stainless steel target frame with 1 cm diameter LC-qTOF: Methanol-rinsed scissor was used to cut 2 2 cm2 pieces of facemasks GC-MS: Methanol-rinsed scissor was used to cut 1.5 1.5 cm2 pieces of material LC-qTOF: 3 times extraction with hot methanol (60-65C) GC-MS: and methanol was added to a final volume of 1500 L. Samples were sonicated for 30 min at 25 C see references in paper see references in paper Clean up na Measurement Thirteen individual PFCs were analyzed using the ion-pairing method. HPLC-MSMS Total fluorine (TF) and extractable organic fluorine (EOF) also were measured in the blood samples using combustion ion chromatography Combustion ion chromatography (CIC), The prevailing assumption has been that all PFASs are incinerated in CIC na and matrix components have no impact on this process The optimal separation was obtained using a Chiralpak QN-AX column with CO2/2- propanol (70/30, v/v) as the mobile phase with a flow rate of 1 mL/min, column temper_x0002_ature was 32C, and BPR pressure was 1800 psi. The resolution (Rs) and reten_x0002_tion time were 0.88 and 130 minutes, respectively The Acquity UPC2 (Waters, Prague, Czech Republic) SFC system used in this study consisted of an Acquity UPC2 binary solvent manager, Acquity UPC2 -FL sample manager, Acquity UPC2 convergence manager, Acquity column manager, isocratic solvent manager, and Xevo na TQ-S detector na na chiral HPLC-MS/MS method was developed for alpha-perfluoromethyl branched PFOS Two Chiralpak QN-AX HPLC columns (2.1 mm I.D. _x0003_ 150 mm each, 5 m particles, Chiral technologies Inc. PA) in tandem with a C18 guard column (4.0 mm I.D. _x0003_ 3 mm, 5 m particles, Phenomenex, Torrance, CA) were used for enantioseparation of 1m-PFOS. Chromatographic conditions were optimized in re_x0002_versed-phase mode on an HPLC-MSMS Isocratic elution was applied and the mobile phase consisted of tetrahydrofuran, 0.2 M formic acid, triethylamine, and water in the ratio 70:20:0.05:10, by volume. Flow rate was 0.12 mL/min and column temperature na was kept at 15 _x0001_C. Injection volume was 2 to 20 L LC-MSMS na EOF Ten microliter (10 L) of sample was injected to HPLC-MS/MS for analysis. Details about instrumental analysis has been described in the SI. The most recent international standard method (ISO DIS21675, 2019) was applied to this na study. Target compounds were extracted and analysed by a previously re_x0002_ported method (Martn et al., 2016). Analytical determination was performed on a 1200 Series LC system (Agilent, USA) coupled to a 6410 Agilent triple quadrupole (QqQ) mass spectrometer (MS). Chromatographic separation was carried out on an Agilent Zorbax Eclipse XDB-C18 Rapid Resolution HT (50 mm 4.6 mm i.d.; 1.8 m particle size) column. An electrospray ionization source op_x0002_erating in negative-ion mode was used Separation was performed by gradient elution with methanol (solvent A) and 5 mM ammonium acetate aqueous solution (solvent B) at a flow rate of 0.6 mL min-1 with the column thermostated at 25 C. The elution program was as follows: 0-20 min, na linear gradient from 28 to 95% of solvent A, held for 2 min online-SPE UHPLC-MS/MS established analytical method for analysis of PFASs in serum, plasma, and whole blood as described by na Poothong et al the same as used in the report "Screening of Poly- and Perfluoroalkyl Substances (PFASs) and Extractable Organic Fluorine (EOF) in Swedish Blood Samples" UPLC-MSMS The mobile phases were methanol (MeOH) and 30:70 MeOH:MilliQ water mixture, both with 2 mmol/L ammonium acetate and 5 mmol/L 1-methylpiperidine as additives [31]. Ultra-short chain compounds (C2- C3) were separated by a supercritical fluid chromatographic system na EOF: combustion ion chromatography (CIC) system ultra-high performance liquid chro_x0002_matography coupled to high-resolution mass spectrometry (UHPLC- HRMS) determination. The full-scan mass data were acquired with a resolution of 50000 FWHM and a mass accuracy better than 5 ppm Chromatographic separation was carried out with a Hypersil Gold column (100 _x0005_ 2.1 mm, 1.9 mm) from Thermo Fisher Scientific (Bremen, Germany). The flow rate used was 300 mL min_x0003_1 and the injection volume was 10 mL. The mobile phase consisted of (A) an 0.1% acetic_x0002_acid aqueous solution and (B) methanol:acetoniltrile (80:20, v/containing 0.1% acetic acid. The gradient was as follows: 0 min (40% B) and held for 2 min. After that, solvent B increased linearly to 80% in 4 min, and to 100% in another 4 min and was kept for 3 min. Finally, solvent B changed to the initial percentage (40%) in 0.5 min and was maintained for 3.5 min to equilibrate the column before na the next injection. The total run time was 17 min were determined in serum and cord plasma using procedures as described by (Kato na et al., 2011). total fuorine (TF), extractable organic fuorine (EOF), identifed organic fuorine (IOF, total concentration of identifed PFAAs quantifed as fuorine) and 11 target PFAAs TF and EOF in serum, nails and hair were determined by cyclic neutron activation analysis (CNAA) (Zhang na et al. 2017). LC-HRMS full MS/dd-MS2, t-SIM/dd-MS2 and SIM experiments Kinetex XB C18 column Mobile phases were water (A) and methanol (B) both containing 2 mM of ammonium acetate. The gradient was initiated with 100% eluent A at 0.05 mL min-1. In 1 min the flow increased to 0.3 mL min-1 and the eluent B increased to 20% maintaining this condition for 2 min. The gradi_x0002_ent continued with linear increase to 70% B in 8 min. This con_x0002_dition was maintained for 4 min following by another linear in_x0002_crease of mobile phase B up to 100% in 6 min. After 5 min, the system returned to 100% A and the flow at 0.05 mL/min in 2 na min (HPLC-MS/MS The analytical column was a Luna 5 m C18(2), 100 2 mm (Phenomenex, CA, USA). The eluents were methanol (mobile phase B) and LC-MS grade water, contain_x0002_ing 10 mM ammonium acetate (mobile phase A) The stationary phase was an ACQUITY UPLC BEH C18 1.7 m, 2.1 100 mm column (Waters Corporation, Milford, MA, USA), and the eluents for the mobile phases were a 70:30 mixture of Milli-Q water and methanol (mobile phase A) and methanol (mobile phase B), both containing 2 mmol/L ammo_x0002_nium acetate and 5 mmol/L n- na methylpiperidine The LC MS system consisted of an Agilent 1290 Infinity II high pressure liquid-chromatography (HPLC) system coupled to an Agilent 6546 quadrupole- time-of-flight mass spectrometer (Q-TOF, Agilent Technologies, Santa Clara, CA). Separations were carried out in an EC_x0002_C18 column (2.1 100 mm, 1.9 m), (Agilent Technologies, Santa Clara, CA), while a second LC C18 column (EclipsePlus-C18, 3.0 50 mm 1.8 m) was placed after pump exit to delay any perfluorinated interferents originating from fluidic system. The mobile phases consisted of water added with 20 mM ammonium acetate (A) and acetonitrile added of 0.1% formic acid (B) with a flow rate of 0.3 ml/min. The gradient was as follows: 3% B at time 0, 25% B at 1 min, 25- 85% B from 1 to 9 min, 85-97% from 9 to 10, isocratic 97% B for 2 min, equilibration at 3% B up to 15 min. The volume of injection was optimized and the final result was 20 l. The Q-TOF instrument was operated in negative na ion mode measuring the extractable organofluorine (EOF) in pooled maternal serum, placental tissue, and cord serum samples The EOF was analyzed using combustion ion chromatography, and the concentrations of known PFAS were determined using ultraperformance liquid na chromatography coupled with a tandem mass spectrometer LC-MS/MS extractable na organofluorine (EOF) with CIC Several Replicate 1 samples (used for target PFAS analysis) required an additional clean-up step with solid phase extraction (SPE), weak anion exchange cartridges The EOF content was measured with a CIC system. Target analysis: ultra performance liquid chromatograph (UPLC) with a mass spectrometer (MS/MS). For ultra-short chain compounds an SFC system was coupled to a MS/MS. GC-MS: strong anion exchange (SAX) solid phase extraction (SPE) Total Fluorine Analysis by Particle-Induced Gamma Ray Emission Nonvolatile PFAS Analysis by Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry (LC-qTOF) Nonvolatile PFAS Suspect Screening Volatile PFAS Analysis by Gas Chromatography-Mass Spectrometry Quantification method Working range (ng/mL) As Matrices na na whole blood surface water and whole-blood na na sample extracts na na serum na na water and human serum samples na na serum na na plasma and whole blood na na hair na na internal standard na hair wipes internal standard na na na na breast milk na na serum and plasma na na na isotope na liver na na serum and placental tissue na na hair pooled maternal serum, placental tissue, and cord serum na na samples na na na isotope dilution method, except for TFA and PFPrA analysis (qualitative) due to the lack of suitable internal standards na whole blood TF-analysis: standard response of the external calibration curve (PFOA) LC-qTOF and GC-MS: isotope dilution method na Face masks Reported levels (ng/mL) five cities (Jintan, Nanjing, Guiyang, Beijing, and Shenyang). PFOS was found to be the dominant PFC ranging from 0.446-83.1 ng/ mL. known PFCs could account for >70% of EOF in samples from Beijing, Shenyang, and Guiyang, whereas known PFCs could only account for 30% of EOF in samples from Jintan na The frequency of occurrence of 1m-PFOS in 10 human sam_x0002_ples were 80% (S/N 10). 1m-PFOS EF ranges from 0.395 to 0.474 in human sera (n = 8), and the average 1m-PFOS EF was 0.443 0.025 na 1m-PFOS was racemic (EF = 0.485_x0001_0.511) nonracemic, with a mean EF ((standard deviation) of 0.432 ( 0.009 quantifiable PFASs accounted for 31-86 % of EOF 0-0,07 ng/mL, 0-45 ng F/mL concentrations of total 11 PFAS in hair varied from below matrixspecific limit of quantification (<0.02 ng/g) to 12 3.78 ng/g. Among 9 PFAS quantified, perfluorohexanesulfonic acid (PFHxS), 13 perfluorooctanesulfonic acid (PFOS), and perfluorooctanoic acid (PFOA) were the 14 predominant compounds. PFCs were detected at concentrations in the range from 0.6 to 15.5 ng/g, being PFHpA and PFOS the ones most frequently detected (86% and 76%, respectively) Polyfluoroalkyl phosphate esters (PAPs) were the predominant PFASs in the hand wipe samples (medians between 0.21 and 0.54 ng per sample) The median of estimated daily intakes via hand-to-mouth and dermal contacts (for hands only) for PFOA were 0.83 and 0.50 pgkg bw-1day-1, average sum PFAS concentrations was 346 ng/ g (from 74.1 ng/g to 715 ng/g). The average EOF concentration was 186 ng F/g and 79% of the EOF was explained by the target analytes. In all samples, perfluoro-n-pentanoic acid (PFPeA), perfluoro-n-octanoic acid (PFOA) and sodium perfluoro-1octanesulfonate (PFOS) were the most frequently detected analytes 0.0021 mg kg_x0003_1 b.w.- day and 0.0029 mg kg_x0003_1 b.w.- day, respectively, for PFOA; and for PFOS the daily intake resulted in 0.0092 mg kg_x0003_1 b.w.- day and 0.01254 mg kg_x0003_1 b.w.- day, respectively. Considering TDI values of 1.5 mg kg_x0003_1 b.w.- day for PFOA and 0.15 mg kg_x0003_1 b.w.- day for PFOS na EOF was the major form of fuorine in serum, accounting for 70-80% of TF. The levels of IOF contributed less than 10% of EOF. Perfuorooctane sulfonic acid (PFOS) was found to be the dominant PFAA with mean concentration of 23 ngmL-1 in serum, 35 ngg-1 in hair and 33 ngg-1 in nail range 0.2-150 ng g - 1 Results showed that performance, in terms of recovery, differed between the extraction methods for different PFAS; different extraction methods resulted in different EOF concentrations indicating that the choice of extraction method is important for target PFAS and EOF analysis. Results of maternal serum samples, analyzed in two different laboratories using two different extraction methods, showed an accordance of 107.6% ( 21.3); the detected perfluoroalkyl acids (PFAAs) in maternal and cord serum samples were in the range of 0.076 to 2.9 ng/mL. The detected PFAS were PFBA (range 0.24- 14.6 ng/g), PFBS (0.496 ng/g), PFOA (range 0.08-0.178 ng/g) and PFOS (<LOQ-0.239 ng/g) he amount of unknown PFAS was estimated between the levels of known PFAS and EOF. The EOF levels ranged from 2.85 to 7.17 ng F/ mL (21 PFAS were quantified) in the maternal serum, from 1.02 to 1.85 ng F/g (23 PFAS were quantified) in the placental tissue, and from 1.2 to 2.10 ng F/mL (18 PFAS were quantified) in the cord serum. An average of 24, 51, and 9% of EOF is unidentified IPE had an average ionization enhancement of 9%, while SPE-WAX showed an average ionization suppression of -1%. SPEWAX showed higher average recoveries for procedural blanks (78%), horse serum (96%) and human serum (95%) in comparison to IPE (69%, 36%, 88%, respectively). The CIC analysis for EOF content was observed to be below MDL (<50 ng/mL F) with some contaminations observed in the procedural blanks. The average EOF concentration in the Ronneby group was 234 ng/ mL F (<107-592 ng/mL F) vs 24.8 ng/mL F (17.6-37.8 ng/mL F) in the control group. This was confirmed by target analysis, which found an average PFAS concentration of 346 ng/mL in the exposed group and 7.9 ng/mL in the control group. Summed PFAS concentrations ranged from 15 to 2900 g/m2 info - validation of the method Limitations Analysis of PFOS standard 10 and 100 ng/mL in MeOH showed 95% (SD: 5%) and 98% (SD: 3%) recovery, respectively. In-house reference material (pig's blood) was analyzed before and after every 10 CIC injections (TF mean: 173 ng F/mL and SD: 13 ng/mL, n ) 10) t na combustion efficiencies of 66-110% RSD was 5% na between-run less than or equal to 2.97, precision (Relative Standard Deviation, RSD, %) within-run less than or equal to 1.83 and between-run less than or equal to 1.41, the Rs precision (RSD, %) of enantiospearation within-run less than or equal to 5.50 and between-run less than or equal to 6.12. na recoveries of 70-101.5% RSDs of 1.22-6.86% na na na Matrix recoveries ranged from 61 to 115 % standard deviations for all batches were between 9 and 15 % recoveries ranging from 89 to 92 % (80 to 90 %) and combustion 500 ng (or 50 ng) of PFOA resulted in 85 to 90 % (83 to 89 %) recoveries. Inter-day performance and reproducibility were monitored by repeated combustions of SRM1957 samples. The relative standard deviations for SRM1957 analysed on different days were less than 18 % (19.4_x0004_ 3.2 ng F mL_x0002_1 ); the quantifiable PFASs represented ,83 % of the EOF na procedural blanks, procedural recoveries and internal standards recoveries 121 DIS21675, 2019) was applied to this study. For quality assurance and quality control, procedural blanks, procedural recoveries and internal standards recoveries for each sample were analyzed. Procedural blanks and recoveries were assessed following the same procedure used for hair sample extraction. Detail values for matrix-specific limits of quantification (MLQ), blank and recovery results has been summarized in the SI (Tables S2-S4). Mean procedural recovery ranged from 79%-91% among PFAS na For each batch of 20 samples analysed (within one day), procedural blank, blank samples spiked na Method recoveries in spiked blank gauze pads were 60-90% while in spiked gauze pads with a commercial hand cream the recovery of internal standards ranged between 50-75% average method accuracy ((the obtained concentration in the spiked sample / the nominal concentration) *100) of 9812% repeatability was calculated to be 12% intermediate precision was 116% na Recovery: 20-92%, RSD: 9-40% na recovery, repeatability, linearity and limit of quantifi_x0002_cation. The obtained recoveries varied between 70 and 120% with a precision (RSD) lower than 25%. The limit of quantification (LOQ) ranged between 1.9 and 19.0 ng g_x0003_1 lipid weight for OPs, and between 0.066 ng mL_x0003_1 and 0.666 ng mL_x0003_1 for PFASs. A breast milk reference material was used in order to check the validated method. na Quality controls included reagent methods blanks comprised of bovine serum as well as calibration standards and quality control samples in bovine serum (ACILA AG, Weiterstadt, Germany). Reproducibility was checked by analysing spiked bovine serum and a native human plasma sample. Recovery rates were 102% for PFOS, 99% for PFOA, 104% for PFHxS, 95% for PFNA and 91% for PFBS. Detection limits (LOD) were calculated as three times the signal/noise ratio of the analytical background noise in the temporal vicinity of the analyte signal. The limit of quantification (LOQ) was determined as twice the LOD and was 0.3 mg/L for PFOS and PFOA in FLEHS II (2007e2011) and in FLEHS III (2012e2015) LOQ was 0.2 mg/L for PFOS, PFOA, PFHxS and PFBS, and 0.1 mg/L for PFNA na The limits of detection (LODs) for TF in serum, hair and nails were 0.058 gmL-1, 0.61 gg-1 and 0.60 gg-1, respectively, while the LODs for EOF in serum, hair and nails were 0.02 gmL-1, 0.21 gg-1 and 0.20 gg-1, respectively. Hair standard sample (GBW07601) was used to assess the accuracy for the TF and EOF measurements. The recoveries of TF and EOF at 2.0 gg-1 and 0.50 gg-1 were 991% and 952%, respectively. The LODs of 11 PFAAs ranged from 0.09 to 0.41 ngmL-1. The recoveries of 11 PFAAs ranged from 83 to 116% in bovine serum, 76% to 137% in hair and 68% to 130% in nails. na Trueness was from 94 to 126% with intra-laboratory reproducibility lower than 20%. na Recovery SPE-WAX: 75%, ion-pair method: 51%, SPE-HLB 59% na The obtained sensitivities (LOQ), linearity and RSD accuracies were respectively in the range of 0.07-0.5 ng/g, 0.1 (or 0.2 or 0.5)-10 ng/g, 1-16% sensitivity, linearity, accuracy, matrix effect and stability The calculated matrix-related effect was comprised from 52% to 119%; stability of processed samples, tested while main_x0002_taining the samples in the autosampler at room temperature for 48 h, were in the range of 45-100% na comparing the PFAS concentrations in the pooled samples with the PFAS concentrations measured in the individual samples additional quality control procedures are described elsewhere na (recovery, matrix effect (ME) in terms of intra-/inter-day repeatability na Every extraction batch included a procedural blank and a quality control (QC) sample. The relative standard deviation (RSD) was below 20% for L- PFOS and L-PFOA for the QC samples (n = 19). The acceptable recovery range for target PFAS was set to 20-150% and it was measured separately for each sample with the use of isotopically labelled standards (recovery standards). Compounds, whose recoveries fell outside of this range, were marked as not quantified (n.q.). The performance and condition of the CIC were monitored with repeated injections of an anion standard solution and blank injections. The repeatability of the CIC system was tested by triplicate analysis of the anion standard solution, resulting in an RSD below 10%. The performance of EOF analysis was verified by participating in an interlaboratory comparison study. na TF analysis: Method accuracy was calculated to be between 96 and 106% and precision was calculated to be 5.4%.2,3 Based on the standard response of the external calibration curve. LC-qTOF: Whole method precision : 1.2-35%, Whole method accuracy: 41-310% GC-MS: Whole method precision : 0.62-11%, Whole method accuracy: 62-140% na LoD (ng/mL) subgro M- geeanseurriecmnaemnte na na LC-MS/MS, CIC 50 ng/mL na CIC na LC-MS/MS ). The detection limit (LOD) calculated from 3/K to be 0.1 ng L-1 na na na LC-MS/MS 10 and 50 pg mL_x0002_1 na LC-MS/MS, CIC na na LC-MS/MS na na LC-MS/MS 0.0045-0.09 ng na LC-MS/MS na na LC-MS/MS na na LC-MS/MS na na LC-MS/MS na na CIC 2-100 pg g-1 na LC-HRMS na na LC-MS/MS na na LC-MS/MS na na CIC na na LC-MS/MS, CIC The LOQ of the EOF analysis ranged from 7.1 to 107 ng/mL F in whole blood LOQ ranged from 6 - 4917 pg/mL for the target analysis na CIC, LC-MS/MS 0.5 - 2.5 g/m2 na PIGE, LC-HRMS, GC-MS Title Target and Nontarget Analysis of Per- and Polyfluoralkyl Substances in Wastewater from Electronics Fabrication Facilities Screening for perfluoroalkyl acids in consumer products, building materials and wastes Perfluoroalkyl and polyfluoroalkyl substances (PFASs) in consumer products in Norway - A pilot study Authors Jacob et al. Becanova et al. Herzke et el. Journal year Environ Sci Technol 2021 Vol. 55 Issue 4 Pages 2346-2356 2021 Chemosphere 2016 Chemosphere 2012 comments (t, nt, o) DOI link targeted and untargeted 10.1021/acs.est.0c06690 10.1016/ j.chemosphere.2016.08.1120045- na 6535/ na 10.1016/j.chemosphere.2012.03.035 PFAS The 25 target PFASs included 11 perfluorocarboxylic acids (PFCAs), seven perfluorosulfonic acids (PFSAs), three fluorotelomer sulfonic acids (FTSs), one perfluoroalkylsulfonamide (FOSA), two polyfluorosulfonamido acetic acid derivatives (N-MeFOSAA and N-EtFOSAA), and perfluoro-2-methyl-3-oxahexanoic acid (GenX). PFPA, PFHxA, PFHpA, PFOA, PFNa, PFDA, PFUnDA, PFDoDa, PFTrDA, PFTeDA, PFBS, PFHxS, PFHpS, PFOS and PFDS PFAS (i.e. C4-C14 PFCAs, C4,C6,C8,C10 PFSAs, 6:2 and 8:2 fluorotelomersulfonates (FTSs), PFOSA, 4:2, 6:2, 8:2, 10:2 FTOH CAS (if available in source) na na na Sampling sample amount used waste waters at 3 positions na 126 samples in four categories: Textiles, Floor coverings, Electrical & Electronic equipment and plastics. All bought in Czech Republic 5 g 30 products in 6 different product groups: waterproofing agents, paint, coated fabrics, non-stick ware, electronics and fire fighting agents. They were purchased from retailers in Norway and Sweden. 1 g Pre- treatment na Materials were crushed, chopped or cut into small pieces Liquid and solid samples were homogenized Extraction na Methanol with the addition of ammonium acetate methanol for ionic compounds and ethylacetate forFTOH Clean up Measurement LC-HRMS on orbitrap (targeted and untargeted) na HPLC-MS non-targeted Following extraction, samples were cleaned up according to the procedures for PFAAs analysis described indetail elsewhere (Karaskova et al., 2016). HPLC-ESI-MS/MS Centrifugation and solvent evaporation, clean up with ENVI-Carb and glacial acetic acid (for ionic PFAS) GC-MS Quantification method Working range (ng/mL) As Matrices na na internal standards na internal standard na waste water Textiles, matierials of wood and composite wood, plastics, foam, air conditioner components. electronic components food contact paper, textile, fire fighting foam, water proofing agents and lubricants, paint, leather, carpets, non-stick ware, printed circuit boards reported levels (ng/mL) info - validation of the method PFBS was quantified at the highest concentration among the samples (8040 ng L-1) The sum concentrations of the target PFASs in the diluted discharge samples from each fab were 623, 394, and 376 ng L-1 sum concentrations of target and nontarget PFASs in the diluted discharge samples from each fab were 1490, 78 700, and 2170 ng L-1 na Textiles: up to 77,6 g/kg Plastics: up to 0,384 g/kg OSB and wood: up to 18,3 g/kg (PFAS found in 14 out of 14 samples) Car interior materials: up to 3535 g/kg The accuracy of method was evaluated using a set of spiked solidblank materials (polyurethane foam (n = 6) and sand matrix blank (n = 10)) As standard procedure, laboratory blanks, method detection limits (MDLs) and recoveries were examined. For each sample, a high resolution full scan spectra was used to control positive detections (typical mass tolerance 50 ppm). No laboratory contamination for any of na the analyzed compound was detected Limitations LoD (ng/mL) subgroup Measurement - generic name na na na LC-HRMS MQL = 0.02 - 0.28 g kg- na 1 na LC-MS/MS na MDLs not reported na GC-MS Title Authors Journal US EPA 537.1 - Determination of Selected Perand Polyfluorinated Alkyl Substances in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS) ISO 25101:2009 - Water quality -- Determination of perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA) -- Method for unfiltered samples using solid phase extraction and liquid chromatography/mass spectrometry. na na US EPA 8327 - Per-and Polyfluoroalkyl Substances (PFAS) Using External Standard Calibration and Multiple Reaction Monitoring (MRM) Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS) na na ASTM D7968-17a - Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) ASTM D7979-20 - Standard Test Method for Determination of Per- and Polyfluoroalkyl Substances in Water, Sludge, Influent, Effluent, and Wastewater by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) DIN 38414-14 - German standard methods for the examination of water, waste water and sludge - Sludge and sediments (group S) - Part 14: Determination of selected polyfluorinated compounds (PFC) in sludge, compost and soil - Method using high performance liquid chromatography and mass spectrometric detection (HPLC-MS/MS) (S 14) na na EPA Draft Method 1633 - Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue Samples by LC-MS/MS US EPA OTM45 - Other Test Method 45 (OTM45) Measurement of Selected Per- and Polyfluorinated Alkyl Substances from Stationary Sources DIN 38407-42:2011 - Standard methods for the examination of water, waste water and sludge na na ISO 21675:2019 - Water quality -- Determination of perfluoroalkyl and polyfluoroalkyl substances (PFAS) in water -- Method using solid phase extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS) na na US EPA 537.1 - Determination of Selected Per- and Polyfluorinated Alkyl Substances in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS) US EPA 533 - Determination of Per- and Polyfluoroalkyl Substances in Drinking Water by Isotope Dilution Anion Exchange Solid Phase Extraction and Liquid Chromatography/ Tandem Mass Spectrometry na na Isolating the AFFF Signature in Coastal Watersheds Using Oxidizable PFAS Precursors and Unexplained Organofluorine Ruyle et al. 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Environmental Science & Technology 2020 Vol. 54 Issue 10 Pages 6009-6020 Contamination Profiles of Perfluorinated Chemicals in the Inland and Coastal Waters of Japan Following the Use of Fire-Fighting Foams Taniyasu et al. Total fluorine, extractable organic fluorine, perfluorooctane sulfonate and other related fluorochemicals in liver of Indo-Pacific humpback dolphins (Sousa chinensis) and finless porpoises (Neophocaena phocaenoides) from South China Yeung et al. Retention performance of three widely used SPE sorbents for the extraction of perfluoroalkyl substances from seawater Brumovsky et al. Development of multi-residue extraction procedures using QuEChERS and liquid chromatography tandem mass spectrometry for the determination of different types of organic pollutants in mussel Alvarez-Ruiz et al. ACS Symposium SeriesVol. 1206 Environmental Pollution 157(1): 17-23. Chemosphere 2018 Vol. 193 Pages 259-269 Analytical and Bioanalytical Chemistry 2021 Vol. 413 Issue 15 Pages 4063-4076 Comparison of total fluorine, extractable organic fluorine and perfluorinated compounds in the blood of wild and pefluorooctanoate (PFOA)- exposed rats: Evidence for the presence of other organofluorine compounds Yeung et al. Analytica Chimica Acta 635 (2009) 108-114 Fluorine Mass Balance Analysis of Effluent and Sludge from Nordic Countries Aro et al. Legacy and emerging per- and polyfluoroalkyl substances (PFASs) in Dagang Oilfield: Multimedia distribution and contributions of unknown precursors Meng et al. ACS EST Water 2021, 1, 9, 2087- 2096 Journal of Hazardous Materials 412. Per- and Polyfluoroalkyl Substances in Outdoor and Indoor Dust from Mainland China: Contributions of Unknown Precursors and Implications for Human Exposure Wang et al. Environ Sci Technol. A sensitive method for simultaneous determination of 12 classes of per- and polyfluoroalkyl substances (PFASs) in groundwater by ultrahigh performance liquid chromatography coupled with quadrupole orbitrap high resolution mass spectrometry Siqi Liu, Muhammad Junaid, Chemosphere Wei Zhong, Youchang Zhu and Volume 251, July Nan Xu 2020, 126327 Long-term trends of Per- and polyfluoroalkyl substances (PFAS) in suspended particular matter from German rivers using the direct total oxidizable precursor (dTOP) assay Gckener et al. Environmental science and technology Digging deep--implementation, standardisation and interpretation of a total oxidisable precursor (TOP) assay within the regulatory context of perand polyfluoroalkyl substances (PFASs) in soil Gckener et al. Environmental Sciences Europe Efficient workflow for suspect screening analysis to characterize novel and legacy per and polyfluoroalkyl substances (PFAS) in biosolids Dickman et al. Nontarget Mass Spectrometry Reveals New Perfluoroalkyl Substances in Fish from the Yangtze River and Tangxun Lake, China Liu et al. Analytical and Bioanalytical Chemistry Environmental science and technology Per- and polyfluoroalkyl substances (PFAS) in commercial composts, garden soils, and potting mixes of Australia Sivaram et al. Environmental advances Ultra-Short-Chain PFASs in the Sources of German Drinking Water: Prevalent, Overlooked, Difficult to Remove, and Unregulated Neuwald et al. Environmental science and technology Levels and Temporal Trends of Trifluoroacetate (TFA) in Archived Plants: Evidence for Increasing Emissions of Gaseous TFA Precursors over the Last Decades Freeling et al. Environ. Sci. Technol. Lett. 2022, 9, 400-405 Extraction and Matrix Cleanup Method for Analyzing Novel Per- and Polyfluoroalkyl Ether Acids and Other Per- and Polyfluoroalkyl Substances in Fruits and Vegetables Meng et al. J. Agric. Food Chem. 2022, 70, 4792-4804 Quality assurance and quality control of solid phase extraction for PFAS in water and novel analytical techniques for PFAS analysis Taniyasu et al. Chemosphere PFAS Analytical Methods Development and Sampling Research EPA United States Environmental Protectin Agency CWA Analytical Methods for Per- and Polyfluorinated Alkyl Substances (PFAS) EPA United States Environmental Protectin Agency EPA United States PFAS Strategic Roadmap: EPA's Commitments to Environmental Protectin Action 2021-2024 Agency online online online Nontargeted Discovery of Novel Contaminants in the Great Lakes Region: A Comparison of Fish Fillets and Fish Consumers Identifying Unknown Fluorine-Containing Compounds in Environmental Samples Using 19F NMR and Spectral Database Matching Baygi et al. Environ. Sci. Technol. 2021, 55, 3765-3774 Environmental Gauthier, Jeremy R.; Mabury, Science & Scott Andrew Technology year Comments 2018 (revised 2020) https://www.restek.com/en/technical-literature-library/articles/ method-guide-for-pfas-analysis/ https://www.restek.com/en/technical-literature-library/articles/ 2009 method-guide-for-pfas-analysis/ https://www.restek.com/en/technical-literature-library/articles/ 2019 method-guide-for-pfas-analysis/ 2014 (2017 https://www.restek.com/en/technical-literature-library/articles/ revised) method-guide-for-pfas-analysis/ 2015 (2020 revised) 2011 na 2021 https://www.restek.com/en/technical-literature-library/articles/ 2021 method-guide-for-pfas-analysis/ https://www.restek.com/en/technical-literature-library/articles/ 2011 method-guide-for-pfas-analysis/ https://www.restek.com/en/technical-literature-library/articles/ 2019 method-guide-for-pfas-analysis/ 2018 (revised 2020) https://www.restek.com/en/technical-literature-library/articles/ method-guide-for-pfas-analysis/ include the analysis of multiple short-chain per- and polyfluoroalkyl 2019 substances (PFAS) that cannot be measured by Method 537.1 2021 na 2019 na 2020 2020 2019 na 2021 targeted and non-targeted 2020 targeted 2018 na 2021 na 2019 na 2021 non-targeted 2019 na 2019 na 2021 na 2018 na 2021 targeted 2019 34 from Brase 2021 2014 na 2021 targeted 2019 non-targeted 2021 na 2019 review 2012 na 2014 na 2021 targeted 2018 na 2019 na 2020 non-targeted 2020 targeted and non-targeted 2021 na 2019 na 2017 na 2019 na 2021 targeted 2016 na 2019 targeted 2020 2021 na 2018 na 2018 targeted 2019 na 2020 targeted 2021 targeted 2018 na 2014 na 2020 targeted 2021 na 2017 na 2019 Reference taken from AlAmin-Review 2020 2021 targeted 2016 na 2019 na 2020 2015 na 2009 na 2018 targeted 2021 targeted 2009 na 2021 na 2021 na 2021 na 2020 2022 na For policy makers, the TOP assay may also allow monitoring of trends of unknown or unidentified PFASs, and thus observing shifts in production, e.g., from legacy to emerging PFASs. In addition, restrictions of precursors can be more extensively controlled 2022 by means of the TOP assay 2022 na In total, the Nt-HRMS method revealed 10 homologous classes of 2018 PFASs in the 7 fish liver samples 2022 Targeted analysis and TOP assay Liquid-chromatography (HILIC and RP) and Gas chromatography (derivatization of TFA, liquid-liquid extraction and headspace GC-MS) 2022 and TOP assay was applied A statistically significant positive trend in the TFA concentration 2022 within the study period was found for most species/sites, 2022 na 2022 interlaboratory ringtrial (ILT) according to ISO21675 (27 labs) 2022 2022 commitments to action 2021 - 2024 -> no discussion about analytic 2022 methods isotopic profile deconvoluted chromatogram (IPDC) is developed for 2021 screening of novel contaminants Use of 19F NMR for the identifaction of PFAS in environmental 2023 samples DOI link na na na 10.1021/acs.est.0c07296 10.1039/c9em00281b 10.1016/j.envpol.2020.115567 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https://www.sciencedirect.com/science/article/pii/S00456 https://www.epa.gov/water-research/pfas-analytical-meth https://www.epa.gov/cwa-methods/cwa-analytical-method https://www.epa.gov/pfas/pfas-strategic-roadmap-epas-c file:///C:/Users/jacobsg/Downloads/Baygi-2021-Nontarget 10.1021/acs.est.3c01220 PFAS HFPO-DA NEtFOSAA NMeFOSAA PFBS PFDA PFDoA PFHpA PFHxS PFHxA PFNA PFOS PFOA PFTA PFTrDA PFUnA 11Cl-PF3OUdS 9Cl-PF3ONS ADONA PFOS PFOA CAS (if available in publication) 13252-13-6 2991-50-6 2355-31-9 375-73-5 335-76-2 307-55-1 375-85-9 355-46-4 307-24-4 375-95-1 1763-23-1 335-67-1 376-06-7 72629-94-8 2058-94-8 763051-92-9 756426-58-1 919005-14-4 1763-23-1 335-67-1  PFOS PFOA N-EtFOSAA N-MeFOSAA PFBS PFDA PFDoA PFHpA PFHxS PFHxA PFNA PFTeDA PFTrA PFUdA PFBA PFPeA PFDS PFHpS PFPeS FOSA 4:2 FTS 6:2 FTS 8:2 FTS PFNS 1763-23-1 335-67-1 2991-50-6 2355-31-9 375-73-5 335-76-2 307-55-1 375-85-9 355-46-4 307-24-4 375-95-1 376-06-7 na na 375-22-4 2706-90-3 335-77-3 375-92-8 2706-91-4 754-91-6 757124-72-4 27619-97-2 39108-34-4 68259-12-1 C4-C14 PFCA, C4-C8 PFSA, PFECHS, FHpPrA, 6:2 FTCA, 8:2 FTCA, 10:2 FTCA, 2H-perfluoro-2- decenoic acid, 2H-perfluoro-2octenoic acid 29420-49-3 3871-99-6 1763-23-1 375-22-4 2706-90-3 307-24-4 375-85-9 335-67-1 375-95-1 335-76-2 2058-94-8 307-55-1 72629-94-8 376-06-7 67584-42-3 812-70-4 70887-84-2 27854-31-5 53826-12-3 PFTreA PFTriA PFDoA PFUnA PFDA PFOS PFNA PFecHS PFOA PFHxS PFHpA PFHxA PFBS PFPeA PFBA FHEA FOEA FDEA FOUEA FHpPA FHUEA 29420-49-3 3871-99-6 1763-23-1 375-22-4 2706-90-3 307-24-4 375-85-9 335-67-1 375-95-1 335-76-2 2058-94-8 307-55-1 72629-94-8 376-06-7 67584-42-3 812-70-4 70887-84-2 27854-31-5 53826-12-3) C4-C10 PFCA C4-C8 PFSA 375-22-4 2706-90-3 307-24-4 375-85-9 335-67-1 375-95-1 335-76-2 375-73-5 355-46-4 1763-23-1 PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTrDA PFTeDA PFBS PFPeS PFHxS PFHpS PFOS PFNS PFDS PFDoS 4:2FTS 6:2FTS 8:2FTS PFOSA NMeFOSA NEtFOSA NMeFOSAA NEtFOSAA NMeFOSE NEtFOSE HFPO-DA ADONA PFMPA PFMBA NFDHA 9Cl-PF3ONS 11Cl-PF3OUdS PFEESA 3:3FTCA 5:3FTCA 7:3FTCA 375-85-9 335-67-1 375-95-1 335-76-2 2058-94-8 307-55-1 72629-94-8 376-06-7 375-73-5 2706-91-4 355-46-4 375-92-8 1763-23-1 68259-12-1 335-77-3 79780-39-5 757124-72-4 27619-97-2 39108-34-4 754-91-6 31506-32-8 4151-50-2 2355-31-9 2991-50-6 24448-09-7 1691-99-2 13252-13-6 919005-14-4 377-73-1 863090-89-5 151772-58-6 756426-58-1 763051-92-9 113507-82-7 356-02-5 914637-49-3 812-70-4  HFPO-DA PFBA PFPeA PFDS PFHpS PFPeS FOSA 4:2 FTS 6:2 FTS 8:2 FTS 10:2 FTS 8:2 FTUCA or FOUEA MeFOSA EtFOSA PFHxDA PFODA 9Cl-PF3ONS ADONA PFNS PFecHS 3:3 FTCA 5:3 FTCA 6:2 FTCA or 6:2 FHEA 7:3 FTCA or FHpPA 6:2 FHUEA PFEESA NFDHA PFMPA PFMBA 11Cl-PF3OUdS N-MeFOSE N-EtFOSE Perfluorododecane sulfonate (PFDoS)4) Sodium perfluoro-1-dodecanesulfonate 8:2 FTA or FOEA 10:2 FDEA (PFDoS)4) PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFBS PFHxS PFOS 375-73-5 2706-91-4 355-46-4 375-92-8 763-23-1 68259-12-1 335-77-3 79780-39-5 754-91-6 31506-32-8 4151-50-2 24448-09-7 1691-99-2 2355-31-9 2991-50-6 757124-72-4 27619-97-2 39108-34-4 120226-60-0 919005-14-4 13252-13-6 756426-58-1 763051-92-9 83329-89-9 151772-58-6 113507-82-7 1260224-54-1 863090-89-5 377-73-1 67584-42-3 70887-84-2 53826-13-4 27854-31-5 70887-88-6 356-02-5 914637-49-3 812-70-4 375-22-4 2706-90-3 307-24-4 375-85-9 335-67-1 375-95-1 335-76-2 375-73-5 355-46-4 1763-23-1  PFOS PFOA N-EtFOSAA N-MeFOSAA PFBS PFDA PFDoDA PFHpA PFHxS PFHxA PFNA PFTeDA PFTrDA PFUnDA HFPO-DA PFBA PFPeA PFDS PFHpS FOSA 6:2 FTSA 8:2 FTSA 8:2 FTUCA 8:2 diPAP N-MeFOSA N-EtFOSA PFHxDA PFOcDA 9Cl-PF3ONS DONA NEtFOSAA NMeFOSAA PFBS PFDA PFDoA PFHpA PFHxS PFHxA PFNA PFOS PFOA PFTA PFTrDA PFUnA 375-73-5 (PFBS), 355-46-4 (PFHxS), 37592-8 (PFHpS), 1763-23-1 (PFOS), 335-77-3 (PFDS), 754-91-6 (FOSA), 31506-32-8 (NMeFOSA), 4151-50-2 (N-EtFOSA), 2355-319 (N-MeFOSAA), 2991-50-6 (N-EtFOSAA), 27619-97-2 (6:2 FTSA), 39108-34-4 (8:2 FTSA), 73606-19-6 (9Cl-PF3ONS), 375-22-4 (PFBA), 2706-90-3 (PFPeA), 307-24-4 (PFHxA), 375-85-9 (PFHpA), 335-67-1 (PFOA), 375-95-1 (PFNA), 335-76-2 (PFDA), 2058-94-8 (PFUnDA), 307-55-1 (PFDoDA), 72629-94-8 (PFTrDA), 376-06-7 (PFTeDA), 67905-19-5 (PFHxDA), 16517-11-6 (PFOcDA), 70887-84-2 (8:2 FTUCA), 67841-1 (8:2 diPAP), 13252-13-6 (HFPO-DA), 919005-14-4 (DONA) 375-73-5 335-76-2 307-55-1 375-85-9 355-46-4 307-24-4 375-95-1 1763-23-1 335-67-1 376-06-7 72629-94-8 763051-92-9 2058-94-8  PFOS PFOA PFBS PFDA PFDoA PFHpA PFHxS PFHxA PFNA PFUdA HFPO-DA PFBA PFPeA PFHpS PFPeS 4:2 FTS 6:2 FTS 8:2 FTS 9Cl-PF3ONS ADONA PFEESA NFDHA PFMPA PFMBA 11Cl-PF3OUdS 763051-92-9 (11Cl-PF3OUdS), 756426-58-1 (9Cl-PF3ONS), 919005-14-4 (ADONA), 13252-13-6 (HFPO-DA), 151772-58-6 (NFDHA), 375-22-4 (PFBA), 375-73-5 (PFBS), 39108-34-4 (8:2FTS), 335-76-2 (PFDA), 307-55-1 (PFDoA), 113507-82-7 (PFEESA), 375-92-8 (PFHpS), 375-85-9 (PFHpA), 757124-72-4 (4:2FTS), 355-46-4 (PFHxS), 307-24-4 (PFHxA), 377-73-1 (PFMPA), 863090-89-5 (PFMBA), 375-95-1 (PFNA), 27619-97-2 (6:2FTS), 1763-23-1 (PFOS), 335-67-1 (PFOA), 2706-90-3 (PFPeA), 2706-91-4 (PFPeS), 2058-94-8 (PFUnA) C3-C13 perfluoroalkyl carboxylates (PFCA), C4-C10 perfluoroalkyl sulfonates (PFSA), Cn (n = 4, 6, 8) perfluoroalkyl sulfonamides, C8 perfluoroalkyl sulfonamide acetates, Cn:2 (n = 4, 6, 8) fluorotelomer sulfonates, and a polyfluoroalkyl ether carboxylate (DONA) with 5 perfluorinated carbons na (PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFHxDA, PFOcDA); PFSAs with peruorocarbon chain length of C4-C10 and C12 (PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFDoDS); and precursors, such as uorotelomer sulfonates (4 : 2 FTSA, 6 : 2 FTSA and 8 : 2 FTSA) and peruorooctane sulfonamide (FOSA). The masslabeled internal standard (IS) included 13C-PFBA, 13C- PFPeA, 13C-PFHxA, 13C-PFOA, 13C-PFNA, 13C-PFDA, 13C- PFUnDA, 13CPFDoDA, 13C-PFTeDA, 13C-PFHxDA, 18O-PFHxS, 13C-PFOS, 13C4 : 2 FTSA, 13C-6 : 2 FTSA, 13C-8 : 2 FTSA, and 13C-FOSA. a reference branched PFOS isomer standard was used, containing 1m-PFOS, 6/2m-PFOS, 3/4/5m-PFOS, and 4.4/ 4.5/5.5-m2-PFOS (brPFOSK0113) na 11 PFCAs (C4 to C14), five PFSAs (C4, C6, C7, C8, C10), the cyclic PFAS PFECHS, four PFECAs and PFESAs (HFPO-DA, ADONA; 6:2 and 8:2 Cl-PFESA), two PFPiAs (6:6 PFPiA, 6:8 PFPiA), three fluorotelomer sulfonic acids (4:2 FTSA, 6:2 FTSA, 8:2 FTSA), and three sulfonamide-containing precursors (FOSA, N-EtFOSE, N_x0002_EtFOSAA). A total of 15 internal standards were used, which included seven isotopically labelled PFCAs (13C4-PFBA, 13C2-PFHxA, 13C4-PFOA, 13C5-PFNA, 13C2-PFDA, 13C2- PFUnDA, 13C2-PFDoDA), three PFSAs (13C3-PFBS, 18O2-PFHxS, 13C4-PFOS), one PFECA (13C3eHFPO-DA), two FTSAs (13C2-4:2 FTSA, 13C2-8:2 FTSA), and two sulfonamide-containing precursors (13C8-FOSA, d9-N- EtFOSE). 13C8-PFOA was used as the injection standard na 14 perfluoroalkyl carboxylic acids (PFCAs; C4-16, C18), 8 perfluoroalkyl sulfonic acids (PFSAs; C4-11), perfluorooctane sulfonamide (FOSA), 3 perfluoroalkane sulfonamidoacetic acids (FOSAA, MeFOSAA, EtFOSAA), 2 chlorinated polyfluorinated ether sulfonates (Cl-PFESAs; 9Cl-PF3ONS, 11Cl-PF3OUdS), ADONA, HFPO-DA (GenX), 3 fluorotelomer sulfonates (4:2, 6:2, and 8:2 FTSAs), and 3 fluorotelomer carboxylic acids (3:3, 5:3, and 7:3 FTCAs). Linear (L) and branched (br) isomers na 1H,1H,2H,2H_x0002_162 perfluorohexanol (4:2 FTOH), 1H,1H,2H,2H-perfluorodecanol (8:2 FTOH) and 1H,1H,2H,2H- perfluorododecanol (10:2 FTOH) perfluorooctanoic acid (PFOA), perfluorodecanoic acid (PFDA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), perfluorohexanesulfonic acid (PFHxS) and potassium PFOS na 24 PFAS with carbon chain lengths of C4-C13 perfluroalkylcarboxylic acids, C4-C10 perfluroalkylsulfonates, FOSA, N-MeFOSAA, N-EtFOSAA, perflurooctanesulfon- (amide & amidoacetic acids) as well as 4:2, 6:2 and 8:2 fluorinated telomer acids na 34 PFASs The standard solution spiked with PFASs comprised 12 PFCAs, 3 PFSAs (per_x0002_fluoroalkane sulfonic acids), 3 PAPs (polyfluoroalkyl phosphate esters), 5 FTCAs (fluorotelomer carboxylic acids), 3 FTUCAs (fluo_x0002_rotelomer unsaturated carboxylic acids), 3 FTSs (fluorotelomer sulfonic acids), 3 FASAs (perfluoroalkyl sulfonamides), and 2 FASAAs (perfluoroalkyl sulfonamide acetic acids). na 4 : 2 FTOH, 6 : 2 FTOH, 8 : 2 FTOH, and 10 : 2 FTOH na 44 native target PFASs and 18 mass-labelled PFASs na 7 perfluoroalkyl sulfonic acids (C4-C10), 11 PFCAs (C4-C14), 6 poly_x0002_and perfluoroether carboxylic and sulfonic acids (PFECAs/PFESAs) and 7 perfluoroalkyl acids na au_x0002_thentic standards (STD) of 20 PFASs na d C2eC12 PFCAs, C4, C6, C8 PFSAs, 8:2 fluorotelomer unsaturated carboxylic acid (8:2 FTUCA), 6:2 FTSA, 8:2 FTSA, dodecafluoro-3H-4,8-dioxanoate (DONA), 6:2 Cl_x0002_PFAES, 8:2 Cl-PFAES, 6:2 diPAP, and 8:2 diPAP. [13C4]- per_x0002_fluorobutanoic acid (PFBA), [13C4]ePFOA, [18O2]- perfluorohexane sulfonic acid (PFHxS), [13C4]ePFOS, [13C2]-8:2 FTUCA, [13C4]- 6:2 diPAP, and [13C4]-8:2 diPAP na eleven PFCAs (C4-C14), ve PFSAs (C4, C6-C8 and C10), four FTSAs (4:2, 6:2, 8:2 and 10:2 FTSA), three (alkyl-)FASAs (FOSA, MeFOSA, EtFOSA), three (alkyl-)FASAAs (FOSAA, MeFOSAA, EtFOSAA), two diPAPs (6:2 and 8:2 diPAP) and two uoroalkyl ethers (PFPEs: ADONA and HFPO-DA) na Fluoride standard solution Anion multi-element standard Perfluorooctanoic acid Perfluoro-n-butanoic acid Perfluoro-n-[1,2-13C2]octanoic acid Perfluoro-n-[1,2-13C2]undecanoic acid Potassium perfluoro-1-butanesulfonate Sodium perfluoro-1-[13C8]-octanesulfonate Sodium perfluoro-1-dodecanesulfonate Sodium 1H,1H,2H,2H-perfluorooctane sulfonate (6:2) N-methylperfluoro-1-octanesulfonamide 2-Perfluorooctyl ethanol (8:2) Sodium bis(1H,1H,2H,2H_x0002_perfluorodecyl)phosphate Perfluorooctylphosphonic acid Potassium 9-chlorohexadecafluoro-3-oxanonane-1-sulfonate 2,3,3,3-Tetrafluoro-2-(1,1,2,2,3,3,3- heptafluoropropoxy)propanoic acid na fluo_x0002_rotelomer olefin (8 : 2 FTO), fluorotelomer acrylates (6 : 2, 8 : 2 FTA), fluorotelomer alcohols (4 : 2, 6 : 2, 8 : 2, 10 : 2, and 12 : 2 FTOH), sulfonamides (NMeFBSA, NMeFOSA, and NEtFOSA), and sulfonamidoethanols (NMeFBSE, NMeFOSE, and NEtFOSE); na hexafluoropropylene oxide dimer acid (GenX), perfluoro-1- butanesulfonate (PFBS), perfluoro-n-octanoic acid (PFOA) and perfluoro-1- octanesulfonate (PFOS) na HFPO-DA na MPFBA Perfluoro-n-[13C4]butanoic acid MPFDA Perfluoro-n-[1,2-13C2]decanoic acid MPFDoA Perfluoro-n-[1,2-13C2]dodecanoic acid MPFHxS Pefluoro-1-hexane[18O2]sulfonate MPFHxA Perfluoro-n-[1,2-13C2]hexanoic acid MPFNA Perfluoro-n-[1,2,3,4,5-13C5]nonanoic acid MPFOA Perfluoro-n-[1,2,3,4-13C4]octanoic acid MPFOS Perfluoro-1-[1,2,3,4-13C4]octane sulfonate MPFUnA Perfluoro-n-[1,2-13C2] undecanoic acid PFAS Perfluoroalkyl sulfonates PFBA Perfluoro-n-butanoic acid PFBS Perfluoro-n-butanesulfonate PFDA Perfluordecanoic acid PFDoA Perfluoro-n-dodecanoic acid PFDS Perfluoro-n-decane sulfonate PFHpA Perfluoro-n-heptanoic acid PFHpS Perfluoro-n-heptane sulfonate PFHxA Perfluoro-n-hexanoic acid PFHxS Perfluoro-n-hexane sulfonate PFNA Perfluoro-n-nonanoic acid PFOA Perfluoro-n-octanoic acid PFOS Perfluoro-n-octane sulfonate PFPeA Perfluoro-n-pentanoic acid na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na nine native (i.e. unlabeled) linear PFCAs (C4-C12), five native PFSAs (C4-C8), three native fluorotelomer sulfonates (4:2, 6:2 and 8:2 FTS), sodium dodecafluoro-3H-4,8-dioxanonanoate (NaDONA), the major and minor components of F-53B (9Cl-PF3ONS and 11Cl-PF3OUdS), GenX (HFPO-DA), three perfluoroether/polyether-carboxylic acids (PF4OPeA, PF5OHxA and 3,6-OPFHpA) and a perfluoroethersulfonate (PFEESA) na perfluorinated compounds: PFOA, PFOS, PFNA, and PFBS, and deuterated internal standards: na perfluoro- butanoic (PFBA), pen_x0002_tanoic (PFPeA), hexanoic (PFHxA), heptanoic (PFHpA), octanoic (PFOA), nonanoic (PFNA), decanoic (PFDA), undecanoic (PFUnA), dodecanoic (PFDoA) and tetradecanoic (PFTeDA) acids as well as the perfluoro- butane (PFBS), hexane (PFHxS) and octane (PFOS) sulfonates na perfluoro-2-propoxipropanoic acid (PFPrOPrA), perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), perfluorohexane sulfonic acid (PFHxS), perfluorooctanoic acid (PFOA), perfluorooctane sulfonic acid (PFOS), perfluorononanoic acid (PFNA) and perfluorodecanoic acid (PFDA) nonafluoro-1- butanesulfonic acid (PFBSa), 2-(perfluorohexyl) ethane-1- sulfonic acid (6:2 FTSA), perfluorotridecanoic acid (PFTrDA) and perfluorododecanoic acid (PFDoA) perfluoroundecanoic acid (PFUnDA), perfluorodecane sulfonic acid (PFDS), pefluoropentane sulfonic acid (PFPS) and perfluorononane sulfonic acid (PFNS) na perfluoroalkyl carboxylates (PFCAs): per_x0002_fluorobutanoate (PFBA; C-4), perfluoropentanoate (PFPeA; C-5), perfluorohexanoate (PFHxA; C-6), perfluoroheptanoate (PFHpA; C-7), PFOA (C-8), perfluorononanoate (PFNA; C-9), PFDA (C-10), perfluoroundecanoate (PFUnDA; C-11), perfluorododecanoate (PFDoDA; C-12), perfluoro_x0002_tridecanoate (PFTrDA; C-13), and perfluorotetradecanoate (PFTeDA; C-14); perfluoroalkyl sulfonates (PFSAs): per_x0002_fluorobutane sulfonate (PFBS; C- 4), perfluoropentane sulfo_x0002_nate (PFPeS; C-5), PFHxS (C- 6), perfluoroheptane sulfonate (PFHpS; C-7), PFOS (C-8), perfluorononane sulfonate (PFNS: C-9), and perfluorodecane sulfonate (PFDS; C-10); precursors: 4:2 fluorotelomer sulfonate (4:2 FtS; C-6), 6:2 fluorotelomer sulfonate (6:2 FtS; C-8), 8:2 fluorotelomer sulfonate (8:2 FtS; C-10), perfluorooctane sulfonamide (FOSA; C- 8), N-methyl perfluorooctane sulfonamidoacetic acid (N- MeFOSAA; C-8), and N-ethyl perfluorooctane sul_x0002_fonamidoacetic acid (N-EtFOSAA; C-8). na Perfluorobutanesulphonic acid (PFBuS, CAS number: 375-73-5), perfluoropentanoic acid (PFPeA, CAS number: 2706-90-3), perfluorohexanoic acid (PFHxA, CAS number: 307-24-4), perfluorohexanesulphonic acid (PFHxS, CAS number: 355-46-4), perfluoroheptanoic acid (PFHpA, CAS number: 375-85-9), perfluorooctanoic acid (PFOA, CAS number: 335-67-1), perfluoro-n- (1,2,3,4 13C4)octanoic acid (MPFOA), perfluoroactanesulphonic acid (PFOS, CAS number: 1763- 23-1), and perfluoro-1-(1,2,3,4 13C4)octanesulphonate (MPFOS), perfluorononanoic acid (PFNA, CAS number: 375-95-1), perfluorodecanoic acid (PFDA, CAS number: 335-76-2) na perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA), perfluorohexanoic acid (PFHxA), perfluoroheptanoic acid (PFHpA), PFOA, perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnDA), perfluorododecanoic acid (PFDoDA), perfluorotridecanoic acid (PFTrDA), perfluorotetradecanoic acid (PFTeDA); 7 PFSAs including perfluorobutanesulfonate (PFBS), perfluoropentanesulfonate (PFPeS), PFHxS, perfluoroheptanesulfonate (PFHpS), PFOS, perfluorononanesulfonate (PFNS) and perfluorodecanesulfonate (PFDS); and 3 PFOS precursors including perfluorooctanesulfonamide (FOSA), N-methyl substituted perfluorooctanesulfonamido acetate (NMeFOSAA), N-ethyl substituted perfluorooctanesulfonamido acetate (N-EtFOSAA) na perfluorobutanoic acid (PFBA); perfluoropentanoic acid (PFPeA); perfluorohexanoic acid (PFHxA); perfluoroheptanoic acid (PFHpA); perfluorooctanoate (PFOA); perfluorononanoic acid (PFNA); perfluorodecanoic acid (PFDA); perfluoroundecanoic acid (PFUnDA); perfluorododecanoic acid (PFDoDA); perfluorotridecanoic acid (PFTrDA); perfluorobutanesulfonate (PFBS); perfluoropentanesulfonate (PFPeS); perfluorohexanesulfonate (PFHxS); perfluoroheptanesulfonate (PFHpS); perfluorooctanesulfonate (PFOS); perfluorodecanesulfonate (PFDS); 4:2 fluorotelomer sulfonic acid (4:2 FTS); 6:2 fluorotelomer sulfonic acid (6:2 FTS); 8:2 fluorotelomer sulfonic acid (8:2 FTS); Nethylperfluorooctanesulfonamide (EtFOSA); N- methylperfluorooctanesulfonamide (MeFOSA); chlorinated polyfluorinated ether sulfonate (6:2F- 53B); na perfluoro-n-butanoic acid (PFBA), perfluoron-pentanoic acid (PFPeA), perfluoro-n-hexanoic acid (PFHxA), perfuoro-n-heptanoic acid (PFHpA), perfuoron- octanoic acid (PFOA), perfuoro-n-nonanoic acid (PFNA), perfuoro-n-decanoic acid (PFDA), perfuoro-n-undecanoic acid (PFUdA), perfluoro-n-dodecanoic acid (PFDoA), perfuoro-n- tridecanoic acid (PFTrDA), perfuoro-n-tetradecanoic acid (PFTeDA), perfuoro-n-hexadecanoic acid (PFHxDA), perfuoro-n- octadecanoic acid (PFODA), potassium perfuoro-1- butanesulfonate (PFBS), sodium perfuoro1-hexanesulfonate (PFHxS), sodium perfuoro-1-octanesulfonate (PFOS), sodium perfuoro-1-decanesulfonate (PFDS na perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluorooctanoic acid (PFOA), perfluorooctane sulfonic acid (PFOS), perfluoroheptanoic acid (PFHpA), perfluorohexanoic acid (PFHxA), and perfluoro-1,10-decanedicarboxylic acid (PFDDA) na perfluorooctanoic acid (PFOA), perfluorooctanesulfonate (PFOS) na PFAA, PFHpA, PFOA, PFOS, PFNA, PFDA, PFBA na PFAS Mix na PFBA PFHxA PFHpA PFOA PFNA PFDA PFUnDA PFDoDA PFTrDA PFTeDA PFBS PFHxS PFOS 6:2 FTS FOSA N-MeFOSE N-MeFOSA N-EtFOSE N-EtFOSA na PFHxA, PFOA and PFOS, PFBS, PFHpA and PFNA na PFOA, TFA, PFPrA, PFBA, PFPeA, PFHxA, PFHpA na PFOS na PFOS na PFOS na PFOS PFOA na PFOS, perfluorohexanesulphonate (PFHxS), perfluorobutanesul- phonate (PFBS), perfluorooctanesulfonamide (PFOSA), perfluoro- decanoate (PFDA), perfluorononanoate (PFNA), PFOA, perfluoro-heptanoate (PFHpA), perfluoroundecanoate (PFUnDA), perfluoro-hexanoate (PFHxA) w na PFOS, PFHxS, PFOSA, N-EtFOSA, PFDoDA, PFUnDA, PFDA, PFNA, PFOA, and PFHpA) na PFPA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFDoDA, PFTrDA, PFBS, PFHxS, PFOS, PFOSA, na PFPeA, PFBS, PFOA, PFDA, PFOS na Potassium salts of perfluorohexanesulfonate (PFHxS), perfluorobutanesulfonate (PFBS), and perfluorooctanesulfonamide (PFOSA) Perfluorononanoic acid (PFNA) was purchased from . PFOA Perfluorohexanoic acid (PFHxA) Perfluoroheptanoic acid (PFHpA), perfluorodecanoic acid (PFDA), perfluoroundecanoic acid (PFUnDA), and perfluorododecanoic acid (PFDoDA) Saturated fluorotelomer carboxylate (8:2 FTCA) and unsaturated fluorotelomer carboxylate (8:2 FTUCA) na total, 73 different PFAS were monitored in this study: perfluoroalkyl acids (PFCAs), perfluoroalkyl sulfonic acids (PFSAs), PFCA precursors and intermediates [mono- and diPAPs, fluorotelomer carboxylic acids (FTCAs), fluorotelomer unsaturated carboxylic acids (FTUCAs), and fluorotelomer sulfonic acids (FTSAs)], PFSA precursors and intermediates [perfluoroalkyl sulfonamidoacetic acids (FOSAAs) and perfluoroalkyl sulfonamido phosphate esters (SAmPAPs)], perfluorinated phosphonic acids (PFPAs), perfluorinated phosphinic acids (PFPiAs), chlorinated polyfluorinated ether sulfonic acids (Cl-PFESAs), perfluoroethylcyclohexanesulfonic acid (PFECHS), 4,8-dioxa-3H-perfluorononanoic acid (ADONA), and HFPO-DA. na twenty-six per- and polyfluoroalkyl substances na na 54 PFASs belonging to 12 classes in groundwater, including 24 perfluorocarbons and 30 precursors 41 Targeted analytes; 13 PFCAs, 8 PFSAs, 3 fluorotelomer sulfonic acids, 6 FOSAs, 3 diPAP and 8 other substances before/after TOP asssay na na na targeted analysis: PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA, PFTeDA, PFPrS, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, 4:2-FTS, 6:2-FTS, 8:2-FTS, FBSA, FOSA, N-EtFOSAA, N-MeFOSAA na na na 38 per- and polyfluoroalkyl substances (PFAS); PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA, PFTeDA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFDS, 4:2-FTS, 6:2- FTS, 8:2-FTS, FHuEA, FOuEA, FDUEA, FOEA, FDEA, FPRPA, FPePA, FHpPA, FOSA, N-MeFOSA, N-EtFOA, FOSAA, N-MeFOSAA, N-Et- FOSAA, F-Et-FOSE, 6:2-diPAP, 8:2-diPAP, 6:2/8:2-diPAP na 43 PFASs were analyzed; TFMS, FAP, NTf2, PFEtS, PFPrA, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA, PFTeDA, PFBS, PFHxS, PFHpS, PFOS, PFDS, 6:2-FTS, HFPO-DA, PFPrS, PFPeS, PFNS, PFDoS, Triflinate, DPOSA, TFA, 2,2,3,3,5,5,6,6-Octafluoro-4-(trifluoromethyl)-morpholine, Dichlorodifluoromethane, 1,1,2,2,3,3-Hexafluoro-1-tri- fluoromethoxy-3-trifluorovinyloxy-propane, 1,1,2,2,3,3,4- Heptafluoro-cycloentane, 2,2,3,3,3-Pentafluoropropanol, HFIP, 2,2,3,3,4,4,5,5-Octafluoropentyl methacrylate, 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctyl acrylate, Trimethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)-silane, 3,3,4,4,5,5,,6,6,7,7,8,8,8-Tridecafluorooctyl methacrylate, Triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)-silane, 1,1,2,2,3,3,4,4,4-Nonafluoro-N-(2-hydroxyethyl)-N-methyl-1- butane-sulfonamide, Trichloro(3,3,4,4,5,5,6,6,7,7,8,8,8-trideca- fluorooctyl)silane na TFA 76-05-1 PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoA, PFTrDA, PFTeDA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, PFMOAA, PMPA, PEPA, HFPO-DA, PFO2HxA, PFO3OA, PFO4DA, PFO5DoA, HydroEVE, ADONA (Na+ salt), Nafion by product 2, NVHOS, 9Cl-PF3ONS, Nafion by product 4, Ne-MeFOSAA, N-EtFOSAA, PFBSA, PFHxSA, PFOSA, 4:2-FTS, 6:2- FTS, 8:2-FTS, 5:3-FTCA, 7:3-FTCA, 6:2-FTCA, 8:2-FTCA, 6:2- FTUCA, 8:2-FTUCA na PFBS, PFHxS, PFHpS, PFOS, PFDS, FOSA, N-MeFOSA, N-EtFOSA, N-MeFOSAA, N-EtFOSAA, 6:2-FTSA, 8:2 FTSA, 6:2 Cl-PFESA, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTrDA, PFTeDA, PFHxDA, PFOcDA, 8:2-FTUCA, 8:2- diPAP, HFPO-DA, DONA, 8:2-FTOH na na na na na na na na (screening) na Sampling sample amount used 8.2.1. The sample handler must wash their hands before sampling and wear nitrile gloves while filling and sealing the sample bottles. PFAS contamination during sampling can occur from a number of common sources, such as food packaging and certain foods and beverages. Proper hand washing and wearing nitrile gloves will aid in minimizing this type of accidental contamination of the samples. 8.2.1. Open the tap and allow the system to flush until the water temperature has stabilized (approximately 3 to 5 min). Collect samples from the flowing system. 8.2.2. Fill sample bottles, taking care not to flush out the sample preservation reagent. Samples do not need to be collected headspace free. 8.2.3. After collecting the sample, cap the bottle and agitate by hand until preservative is dissolved. Keep the sample sealed from time of collection until extraction 250-mL Take, preserve and handle samples as specified in ISO 5667-1. For sampling, use thoroughly cleaned bottles . Fill the bottle only to the shoulder with the water to be sampled (approximately 1 000 ml). In the presence of free chlorine, immediately add approximately 80 mg of sodium thiosulfate pentahydrate or another suitable dechlorinating agent (e.g. sodium sulfite). nearest 1 g Grab samples are collected in polypropylene containers. Other types of container materials, such as high-density polyethylene (HDPE), may be used if performance is acceptable for the project. PTFE containers and contact surfaces with PTFE should be avoided. Depending on the needs of the project, field blanks may be required and should be collected according to recommended PFAS sampling practices, where available. The samplers should acquire pre- verified reagent water and containers from the analytical laboratory for preparing field blanks, where practical. Aqueous field samples and associated QC samples must be collected in separate containers, including field blanks, MS/MSDs, and duplicates. Volumes collected for water samples should match volumes consumed in the laboratory's preparation procedure. Conventional laboratory practices involving chain of custody, field sampling, laboratory custody beginning with receipt and transfer custody, and sampling protocols should be followed. na Grab samples are collected in glass or polypropylene containers. Sample containers and contact surfaces with PTFE shall be avoided. 2 g Grab samples are collected in polypropylene containers. Sample containers and contact surfaces with PTFE shall be avoided. 5-mL sample size per analysis According to DIN 38402-24, DIN 38414-11, DIN EN ISO 5667- 13 1 0,01 g received by the laboratory within 48 hours of collection. The laboratory must confirm that the sample temperature is 0 - 6 C upon receipt. Once received by the laboratory, the samples must be stored at -20 C until sample preparation. 8.3 Solid (soil, sediment, biosolid), excluding tissue 8.3.1 Collect samples as grab samples using wide-mouth jars and fill no more than full (see Section 6.1.1.2 for container size and type). 8.3.2 Maintain solid samples protected from light (in HDPE containers) at 0 - 6 C from the time of collection until receipt at the laboratory. The laboratory must confirm that the sample temperature is 0 - 6 C upon receipt. Once received by the laboratory, the samples must be stored at -20 C until sample preparation. 8.4 Fish and other tissue samples The nature of the tissues of interest may vary by project. Field sampling plans and protocols should explicitly state the samples to be collected and if any processing will be conducted in the field (e.g., filleting of whole fish or removal of organs). All field procedures must involve materials and equipment that have been shown to be free of PFAS. 8.4.1 Fish may be cleaned, filleted, or processed in other ways in the field, such that the laboratory may expect to receive whole fish, fish fillets, or other tissues for analysis 8.4.2 If whole fish are collected, wrap the fish in aluminum foil or food-grade polyethylene tubing, and maintain at 0 - 6 C from the time of collection until receipt at the laboratory, to a maximum time of 24 hours. If a longer transport time is necessary, freeze the samplebefore shipping. Ideally, fish should be frozen upon collection and shipped to the laboratory on dry ice. 8.4.3 Once received by the laboratory, the samples must be maintained protected from light at -20 C until prepared. Store unused samples in HDPE containers or wrapped in aluminum foil at -20 C Aqueos samples: Typical sample size is 500 mL; however, sample size may be up to 1000 mL, Solid samples: The maximum sample weight for sediment or soil is 5 g dry weight. The maximum sample weight for biosolids is 0.5 g dry weight. The default sample weight for tissue is 2 g wet weight; however, a 1-g sample may be used. This method involves collection and recovery of trace concentrations of semivolatile organic compounds. Therefore, field sampling and recovery staff must be trained in the best practices for handling and using organic solvents in field environments to recover and protect samples from contamination. 3.0 dry standard cubic meters of source gas Take samples as specified in DIN 38402-11, DIN 38402-12, DIN 38402-13, DIN 38402-15 and DIN ISO 5667-5 Use only cleaned vessels for sampling and fill them completely with the water sample na Take, preserve and handle samples as specified in ISO 5667-1 and ISO 5667-3. Weigh the sample bottle with its original cap and water sample, to the nearest 1 g or mark the line on the sample bottle with the sample volume. 1 g 8.2.1. The sample handler must wash their hands before sampling and wear nitrile gloves while filling and sealing the sample bottles. PFAS contamination during sampling can occur from a number of common sources, such as food packaging and certain foods and beverages. Proper hand washing and wearing nitrile gloves will aid in minimizing this type of accidental contamination of the samples. 8.2.1. Open the tap and allow the system to flush until the water temperature has stabilized (approximately 3 to 5 min). Collect samples from the flowing system. 8.2.2. Fill sample bottles, taking care not to flush out the sample preservation reagent. Samples do not need to be collected headspace free. 8.2.3. After collecting the sample, cap the bottle and agitate by hand until preservative is dissolved. Keep the sample sealed from time of collection until extraction 250-mL Open the tap and allow the system to flush until the water temperature has stabilized. Collect samples from the flowing system. Samples do not need to be collected headspace free. After collecting the sample, cap the bottle and agitate by hand until the preservative is dissolved. Keep the sample sealed from time of collection until extraction. 100-250 mL na na surface water and aquatic invertebrates na River water in China and Germany na Marine mammal liver samples na river, sea, waste and effluent waters 10 g river water na na na na water from firefighting run into a creek na water from DWTP na pump stations around a firefighting training area na na na water, sediments and biota (including biofilm, invertebrates and fish na na na Sorbent-impregnated polyurethane foam (SIP) disc passive air samplers were therefore deployed for 3 months na Tap water, lake water, bottled water and river water sam_x0002_ples were evaluated in this study. According to EPA guidelines in Method 533 1.5 mL na na na na 2 L river water samples river water na na na 500 mL na na na na dated cores of sediment na per_x0002_fluorooctanoic acid (PFOA), perfluorohexyl sulfonate potassium (PFHSK), perfluorinated butyl sulfonic acid potassium (PFBSK), perfluoro-1-octanesulfonyl fluoride (PFSF), nonafluorobutane-1-sulfonic acid (OSA) na In total, 16 Water samples (12 L) were collected from the Uppsala- Stockholm region in Sweden in March to April 2015 flocculation with Al2(SO4)3, sand filtration, GAC fil_x0002_tration (Norit 830W, five years since last regeneration), and disinfection with UV and chloramine (NH2Cl). Two tap water samples Three samples were also collected from a pilot-scale treatment plant that takes water from after sand filtration in the full_x0002_scale DW Triplicate samples were collected downstream from the major waste_x0002_water treatment plant (WWTP) na na na sampling process lasted for 48 h with a flow rate of 20 Lmin-1 na Eighteen sampling sites were selected based on land use, proximity to primary contaminant 74 sources na na na na na na na bird eggs, fish, marine mammals, terrestrial mammals, surface water, WWTP effluents and sludge, and air na free ranging chickens feathers small pieces of approximately 1 mm na Effluent samples (n 12) were collected in duplicate from six STWs along three rivers in the south east of England Runoff samples were collected from grass field drainage (n 3) and street runoff (n 2) during periods of rainfall Grab samples were collected (200 mL) in amber glass bottles. na na na influent and effluent water from a drinking water treatment plant na Dust from fire stations na drinking waters (DW), 12 ground waters (GW), 13 surface waters (SW), 8 influents and 11 effluents of wastewater treatment plants 100 l fish muscle tissue 1g 24-h composite flow-proportional samples were collected from different places within an advanced drinking water treatment plant (DWTP) The raw water was subjected to primary treatment by coagulation, flocculation, and sedimentation and secondary treatment by granular activated carbon (GAC) filtration. In addition, three grab samples were collected from Changzhou wastewater treatment plant effluent, SW, and tap water system to investigate the occurrence of the EOCs within the complete water/wastewater environment. Within 72 h of collection, samples were passed through a 0.7-m glass fiber filter. The filtrate pH was adjusted to 10 with ammonium hydroxide, and then a mixture of the isotopically-labeled surrogates (IS) were spiked at a final concentration of 25 ng L-1 . Prior to preparation and analysis, all samples were kept at 4 C in the dark na lyophilized na na na Commercial POCIS with HLB (hydrophilic-lipophilic balance) phase were supplied by Environmental Sampling Technologies. Home-made POCIS were assembled using HLB sorbent phase (60 m particle size), and 0.1 m pore size polyethersulfone (PES) membranes. PES membranes were washed before assembling in a H2O/CH3OH solution (80:20 v/v) for 24 h and then with CH3OH for 24 h Four samplers were exposed in the influent and four in the effluent of Site 1; two of these were re_x0002_trieved after for 14 days, while the other two after 28 days na Surface waters and effluent wastewater samples, collected from different sampling points na na na Water, sediment and biota (polychaetes, pelagic zooplankton, crabs, fish, glaucous gulls) samples were collected from locations impacted by a firefighting training site (FFTS) and a landfill as well as from a reference site; Polychaetes were depurated overnight in seawater in order to separate sediment-bound PFAS from accumulated PFAS. water in 1L aluminum bottles (methanol cleaned), frozen 1 L na na na na Grab DW samples from different sources, namely tap water (n = 13), fountain water (n = 5), and well water (n = 5), were collected at the end of May 2015 Before SPE, samples were acidified with sulfuric acid (pH 3), and sodium thiosulfate was added to each sample (30 mg L-1 ) to reduce any residual chlorine that might be added as a disinfectant na The surface water samples were first centrifuged at 4500 g to separate solid particles and then filtered off with 0.45 m pore size membrane to remove suspended particles. The samples were heated in oil bath at 105 C for 30 min then stored at 4 C for further use na plants were cultured with PFOS and PFOA spiked solution Longitudinal and cross sections of fresh plant roots at the root hair zone and stem sections 10 cm above the root collar or crown were made na surface water na liver samples of Indo-Pacific humpback dolphins na na mussels na na na The effluent and sludge samples were collected in low-density polyethylene (LDPE) containers na na na outdoor and indoor dust na The German ESB collects SPM in the rivers Rhine, Elbe, Danube, Saar, Saale and Mulde na na na grab samples of PS (n = 3) and WAS (n = 3) from a wastewater treatment plant (WWTP) were collected in polypropylene (PP) bottles (250 mL) na A total of three fish species were obtained at the Yangtze River site, including common carp (Cyprinus carpio), silver carp (Hypophthaimichthys molitrix), and bighead carp (Aristichthys nobilis). The same three species were obtained at Tangxun Lake as well as a fourth species, white Amur bream (Parabramis pekinensis) na A total of 19 commercially available garden products comprising four composts, two garden soils, and thirteen potting-mixes were purchased in 2020 in Newcastle, Australia 2 gram 46 grab water samples were obtained from 13 water suppliers all over Germany, all representing direct or indirect source waters for drinking water production. These comprised 16 surface water samples, 16 bank filtrate samples, 7 raw water samples, and 7 groundwater samples, covering the river basins Danube, Elbe, Ems, Havel, Main, Neckar, Rhine, and Sieg, among others, and their surroundings 200 g for LC and 19 mL for GC Freeze-dried, homogenized, and finely ground plant material 0.25 gram total of 10 types of fruits and vegetables were purchased from Whole Foods Market (Raleigh, NC, U.S.A.) in January 2019 Samples were stored at 5 3 C in the dark until analysis na 1) EPA Technical brief on PFAS methods and Guidance for sampling and analyzing water and other Environmental media 2) EPA methods 533 and 537.1 3) iTRC sampling and analylitical methods 4) Michigan Department of Environmental quality General PFAS sampling Guidance 5) New Jesey Department of environmental protection PFNA/ PFAS sampling information for Water systems 6) New York department of Environmental conservation guidelines for sampling and analysis of PFAS 7) North East Biosolids and Residuals Association (NEBRA) sampling and analysis of PFAS in biosolids and associated media na na na na na Fish fillet and sera cohort collection and storage were described by Renaguli et al. 0.5 gram Pre- treatment na without pretreatment, homogenize the sample by shaking Samples are prepared using an appropriate sample preparation method (e.g., solvent dilution or extraction). na Standards and samples shall be in a 50:50 methanol:water solution containing 0.1 % acetic acid. When preparing the sample, observe the specifications of the Sewage Sludge Ordinance (AbfKlrV) and the Federal Soil Protection Ordinance (BBodSchV). A sufficiently homogeneous laboratory sample must be available for taking a partial sample (test sample). Observe the specifications according to DIN 19747 for taking partial samples. The sample must not be dehydrated before homogenization, e.g. by centrifugation, as the soluble fraction of some PFCs cannot be neglected. Homogenize water sediments and thin-bodied sewage sludges by stirring and take a subsample, if necessary with continued stirring. For soil, compost, pressed sludge and animal feed, reduce laboratory sample according to DIN 19747, e.g. by means of cross-rugation divider (8.6). Sort out foreign materials and record gravimetrically; if necessary, examine these materials separately. Take a partial sample and dry it; measure the partial sample in such a way that, if possible, at least a dry mass of 5 g can be expected. The subsample must be representative of the laboratory sample and, for soil samples, should be at least 1/4 of the mass of the laboratory sample. In the case of homogeneous, finegrained and free-flowing materials, the subsample may be less. Preferably freeze-dry sewage sludge according to DIN 38414-22 (8.5), other samples if necessary at 40 C in a drying oven, depending on the water content. Translated with www.DeepL.com/Translator (free version) na Particular matter filter The samples are analysed in the unfiltered state. The pH value of the sample should lie in the range between pH 6 and pH 8 and shall be adjusted with sodium hydroxide solution or sulfuric acid, if necessary samples are analysed without pre-treatment na na were extracted following the methods described in prior work SPE according to the ISO/ DIS 25101:2009 method using Oasis weak anion exchange (WAX) Glass microfiber filters, Solid phase extraction (SPE) was performed as described previously (Joerss et al., 2019). extraction using the 129 procedure described by Powley et a sonication, Oasis weak anion exchange cartridges SPE following the pro_x0002_tocol previously described by Lockwood et al. Fresh plant samples (roots, stems and leaves) in both the blank 140 and treatment groups were freeze-dried with a freeze dryer (Biocool FD-2A, Beijing, China) and 141 homogenized with a micro plant grinding machine solid-phase extraction (SPE) n (SPE) based on earlier literature (Coggan et al., 2019a). were pre-treated according to previously reported methodology (Boone et al., 2019; Eschauzier et al., 2012; Post et al., 2013). PresepC-Agri (C18) cartridges (Wako, Japan) and Oasis HLB cartridges unfiltered precipitation samples were oxidized using a previously developed TOP assay method solid-phase extraction (SPE) using Oasis WAX cartridges Biota samples were freeze-dried, ground and homogenized prior to analysis. Sediments were also freezedried, sieved at 2 mm and homogenized. Biota samples were processed using a previously published method extraction and SPE-WAX sequential cold-column extraction solid phase microextraction (SPME), hydrophiliclipophilic balance-weak anion-exchange/polyacrylonitrile (HLB-WAX/PAN) as a SPME coating na extraction and Envi-Carb na SPE filtered and TF, SPE na na lyophilized, and homogenized, fortified with surrogate standard extracted by repli_x0002_cates of MTBE. Samples were cleaned using Envi Carb 300 L of analytical identification material solution (0.015 mg/mL) and 100 L of reference material so_x0002_lution (0.06 mg/mL) were mixed The water was then extracted using the HLB and ENV car_x0002_tridges. The 12-L samples collected during field sampling were filtered using glass fiber filters One subsample was ex_x0002_tracted using the 1 g Oasis HLB cartridge and the other using the 1 g Bond-Elut ENV cartridge AutoAD SPE ultrasonically extracted extraction with Oasis MAX, Oasis MCX and Oasis HLB cartridges 0.5 g pre-cleaned micro glass beads (Filter Aid 400, 3M, MN) were added to solid phase extraction 85 (SPE) cartridges (200 mg, 6 mL Oasis HLB, Waters, MA) sorbent cartridge was made with a 1 mL polypropylene syringe packed with 80 mg sorbent and quartz wool plugged in the end Analyte isolation and pre-concentration from water samples is car_x0002_ried out by off-line Solid Phase Extraction (SPE) as described previously (Masi et al., 2013). na detailed description per sample type in publication na Solid Phase Extraction (SPE) of 200 mL sample water was carried out using Phenomenex Strata-X cartridges preconditioned with 3 mL 50:50 acetonitrile/acetone (v/v), washed with 3 mL HPLC_x0002_grade H2O and loaded at a rate of 5 mL/min. Loaded cartridges were dried under vacuum for 15 min and eluted with 2 _x0003_ 7 mL aliquots of 50:50 acetonitrile/acetone (v/v) at a rate of 1 mL/min. Extracts were evaporated to dryness using rotary evaporation and reconstituted with 1 mL of (80:20 HPLC H2O/acetonitrile, v/v) spiked with internal standards to 25 ng/mL micro-SPE the optimal phase consisting of a 50:50 mixture of C18 and aminopropyl silica samples were filtered with regenerated cellu_x0002_lose (RC) syringe filters 0.45 m na NO Solid phase extraction (SPE) by WAX cartridges and then freezing at -30 C An automated Agilent 1260 Infinity Flexible Cube was employed to achieve online preconcentration of all analytes. The system consisted of a quaternary pump with four solvent lines used to transfer samples to SPE columns via two 10-port switching valves. Two SPE columns were alternatively used during the analytical cycle. In addition, a delay column (Agilent Eclipse Plus C18, 4.6 50 mm, 3.5 m) was installed after the mixing valve of the quaternary pump and before the autosampler to minimize potential PFAS interferences from the solvent system automated solid phase extraction using a commercially available weakly basic secondary and tertiary ammonium polymeric anion exchange sorbent na na 200 mL of surface or wastewater sample (pH 7) were passed through an Oasis HLB SPE cartridge (200 mg) previously conditioned with 4 mL of methanol and 8 mL of Milli-Q water. After loading the sample, the elution was performed with two aliquots of 4 mL of MeOH. The extract collected was evaporated under a gentle nitrogen stream using a Turbo Vap LV from Zymark (Hopkinton, MA), with a water bath temperature of 37 C and a N2 pressure of 15 psi. Finally, the residue was re-dissolved in 1 mL of MeOH/water (20:80), achieving a final preconcentration factor of 200:1 The LC-MS/MS system was equipped with an on_x0002_line solid phase extraction system (Thermo Scientific EQUAN MAX) allowing for injection volumes from 0.5 to 5.0 mL. After injection, the sample was loaded onto the solid phase extraction trap car_x0002_tridge (SPETC). The sample was then rinsed with deionized water to remove preservatives and buffer salts, before engaging a switch_x0002_ing valve to reverse the direction of mobile phase flow to enable elution of the SPETC onto the analytical column. Elution of the an_x0002_alytes from the SPETC was performed using a basic mobile phase of deionized water and methanol modified with ammonium hy_x0002_droxide (0.1 to 1% in both eluents) and a flow rate of 250 to 300 L/minute. add IS, SPE Oasis HLB, evaporate to dry and reconsitute in mobile phase A na Extraction experiments for the spiked samples with different PFOS concentrations (5-200 ng/L-1 ) were con_x0002_ducted under the optimized conditions. Briefly, 100 mL of water sample or 50 mL pretreated human serum sample was added into a polypropylene flask (pH = 3), 100 mg of MIPDA@Fe3O4 was added to the solution, and the mixture was sonicated for 2 min. Then the solution was transferred to a thermostatic bath and agitated at 150 rpm (298 K) for 30 min, to facilitate mass transfer and adsorption of the PFOS onto MIPDA@Fe3O4. The MIPDA@Fe3O4 was isolated using an external magnetic field and the supernatant was discarded. Then the col_x0002_lected magnetic adsorbents were transferred to a 50 mL polypropylene flask, with 10 mL methanol added as a des_x0002_orption solvent. The mixture was shaken in a thermostatic bath (150 rpm, 298 K) for 10 min and the eluent was then dried under a gentle nitrogen The vacuum extraction and drying devices LiChrolut used for SPE procedure SPE optimization was performed by com_x0002_paring Oasis HLB, MCX, and MAX cartridge na Extraction of the target compounds PFOA and PFOS was based on 147 previous methods with small modifications. solid phase extraction by Oasis WAX cartridges and Oasis HLB cartridges e ion-pairing method, the details of which are described elsewhere (Hansen et al., 2001), the best overall extraction conditions were found to be at pH 8 and 50%/100% matrix seawater content using Oasis HLB/StrataTM-X as SPE sorbents and methanol as eluent (i) SQ and EMR_x0002_Lipid, (ii) AQ and Z-sep+ bulk-based dSPE and (iii) AQ and graphitized carbon black (GCB)-based dSPE PFCs were extracted using the ion-pair method and two-step clean-up procedure using Envi-carb and WAX SPE, as described elsewhere SPE na ultrasonic extraction described in our previous study Groundwater samples were treated according to a previously validated methodology for PFASs (Boone et al., 2014) SPM is collected every month by sedimentation traps installed in about 1 m depth in the water stream of the river or in a partial stream that runs through a measuring station na samples were lyophilized, pulverized The whole liver was collected from each individual fish, weighed (wet liver weight), and placed into a clean polyethylene bag. All liver samples and 10 g of potassium chloride granules were freezedried, weighed homogenized, freeze-dried, ground and sieved (2 mm) composts, potting mixes, and garden soils na na Samples were taken out of the original packages and stored in zip bags (polyethylene, Ziploc) at -20 C before analysis. NA na na na homogenization of fish fillet or serum Extraction S-DVB Solid Phase Extraction SPE (WAX, HLB, C18) Direct Injection Vortexing and shaking with 50:50 MeOH/water and 50:50 MeOH/water/ NH3 (pH 9-10) Direct Injection Sonication with MeOH SPE (aqueos samples), methanol (solids), extracted in potassium hydroxide and acetonitrile followed by basic methanol (tissue) Sampling Train with XAD resin and impingers WAX (weak anion exchange) Solid Phase Extraction (Use at least 60 mg of the solid phase material (7.3) for a sample volume of e.g. 50 ml) WAX (weak anion exchange) Solid Phase Extraction S-DVB Solid Phase Extraction WAX (weak anion exchange) Solid Phase Extraction na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na methanol 100% 24 h at room t na na na na na na na na na na na na Sediment and biota samples were extracted with methanol. Water and melted snow samples were extracted on Oasis Waters (Mildford, MA, USA) weak-anion exchange (WAX) SPE cartridges (6 mL volume, 0.5 g). na SPE na na na na na na na na na na na Sample extraction with methyl tertbutyl ether and tetrabutylammonium hydrogensulfate na Two extraction solvents were used, (A) aqueous acetic acid (1% v/v) and (B) 90:10 (v/v) ethanol:aqueous acetic acid (1% v/v). A series of ultrasonication solvent extractions were used All of the fish samples with the procedural blank salts were extracted with acidified acetonitrile The samples were extracted with methanol/ 200 mM ammonium acetate mixture by shaking and vortexed for 5 min. The PP tubes were then placed in an ultrasonic water bath for 20 min at 30C and then centrifuged for 20 min at 4000 g. The supernatant was transferred to another PP tube, and the samples were extracted three times. The extracts were evaporated to dryness under N2 gas and reconstituted with 1.5 mL of a 99:1 (v/v) methanol/glacial acetic acid mixture. for GC: headspace extraction or liquid-liquid extraction Plant material was spiked with a defined amount of IS and mixed with 0.8 mL of MeOH and 0.8 mL of ultrapure water (+1% (v/v) formic acid). The obtained suspension was agitated for 15 min using a reciprocating shaker and sonicated for another 15 min. After centrifugation (15 min, 4695g), the supernatant was transferred to another 15 mL PP centrifuge tube. This procedure was repeated twice with fresh extractant to optimize the extraction yield After spiked standards were allowed to equilibrate with individual food matrices for 12 h, 4 mL of basic methanol was added for extraction, followed by vortexing for 30 s, sonicating for 30 min, and centrifuging at 4000 rpm for 10 min. The 12 h equilibrium time was selected on the basis of previous studies. The supernatant was decanted into clean 15 mL polypropylene tubes. After 3 extraction cycles, 13 mL of supernatant (first supernatant) was collected for each sample. The extracts were stored at -20 C for 12 h to precipitate any starch present and then centrifuged at 4000 rpm for 10 min to separate solids. na na na na A set of 11 isotope-labeled PFAS (listed in Table S.1) was added as surrogate recovery standards to 0.5 g of homogenized matrix (fish fillet or serum) prior to extraction with 3 mL of methanol followed by ENVI-Carb activated carbon powder cleanup. Clean up Concentrate the extract to dryness under a gentle stream of nitrogen in a heated water bath (60-65 C) to remove all the water/methanol mix. Add the appropriate amount of 96:4% (vol/vol) methanol:water solution and the IS PDS to the collection vial to bring the volume to 1 mL and vortex. Add 4 ml of acetate buffer solution to the dried cartridge and discard the eluate. Then elute the target analytes with 4 ml of methanol, followed by 4 ml of 0,1 % ammonia/methanol (5.9) at a rate of one drop per second. Evaporate the eluate with a gentle stream of nitrogen gas (5.11) to a final volume of 500 l. Sample cleanup - Cleanup procedures should not be necessary for relatively clean sample matrices. Extracts from highly contaminated environmental, waste or biota samples may require additional cleanup steps prior to analysis to meet acceptance criteria for all QC categories. The specific cleanup procedure used will depend upon the analytes of interest, the nature of the interferences, and the DQOs for the project. At the time of publication, no cleanup methods have been validated in conjunction with this determinative method. na na SPE WAX (optional) Elution with MeOH 0.1% NH3 Carbon (aqueos samples), SPE (solids), carbon and SPE (tissue), Carbon cleanup may remove analytes if the sample has a very low organic carbon content (this is unusual for non-drinking water environmental samples). If the laboratory can demonstrate that the carbon cleanup is detrimental to the sample analysis (by comparing results when skipping the carbon cleanup during reanalysis), then the carbon cleanup may be skipped for that specific sample Concentrate the eluate to dryness, e.g. in a nitrogen stream. Dissolve the residue in e.g. 1 ml using a mixture of solvent and water in accordance with the composition of the reference solutions. If necessary, filter the extract through a syringe filter and use a partial volume for the analysis. Add water/ acetate buffer, centrifuge, evaporate Concentrate the extract to dryness under a gentle stream of nitrogen in a heated water bath (60-65 C) to remove all the water/methanol mix. Add the appropriate amount of 96:4% (vol/vol) methanol:water solution and the IS PDS to the collection vial to bring the volume to 1 mL and vortex. The extract is concentrated to dryness with nitrogen in a heated water bath. The extract volume is adjusted to 1.0 mL with 20% water in methanol (v/v), and three isotopically labeled isotope performance standards are added. na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na Clean-up of methanol extracts was conducted using active carbon (EnviCarb, Sigma_x0002_Aldrich Co., PA, USA) na na na na na na na na na na na na na na na na SPE (solid phase extraction) combined with GCB (Graphitized carbon black) purified with weak anion exchange cartridges (SPE solid phase extraction) The mixture was then transferred into 2 mL microcentrifuge tubes prefilled with 25 - 40 mg Envicarb carbon. The extracts were then vortexed for 30 sec, centrifuged for 20 min at 14,000 g, and 500 L of supernatant was transferred into a 1.25 mL PP LC-MS vials. for LC: multilayer solid-phase extraction (mlSPE) or weak anionexchange SPE (solid phase extraction) na To clean up food extracts, the secondary supernatant was diluted with 140 mL of deionized water and then loaded onto Oasis WAX SPE cartridges SPE in-situ SPE purge and trap extraction na na na na Measurement LC-MS/MS (capable of negative ion electrospray ionization (ESI)) HPLC-MS/MS LC-MS/MS UPLC-ESI(-)-MS/MS LC/MS/MS HPLC-ESI(-)-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS n the electrospray ionization (ESI) negative mode LC-MS/MS (capable of negative ion electrospray ionization (ESI)) LC-MS/MS (LC-MS/MS multivariate clustering techniques EOF homologue, isomer and extractable organofluorine (EOF) profiling LC-MSMS source-specific fingerprints of per- and polyfluoroalkyl substances (PFASs) in river water from China and Germany The TOP assay was performed according to Houtz and Sedlak (2012) LC-MSMS f targeted PFAS analysis, EOF and total fluorine determination, and suspect screening UPLC MS/MS (targeted analysis) and UPLC-Orbitrap-MS (suspect screening) EOF by combustion ion chromatography (CIC) combusted directly on the CIC for determination of total 120 fluorine (TF) Suspect screening by LC-orbitrap and feature extraction high-resolution graphite furnace continuum source molecular absorption spectrometry (HR- MAS) 400 g of W was used as a permanent modifier together with an optimised temperature program UPLC-IMS-QTOF-MS, combination of mass defect analysis with common fragment and neutral loss filtering AC_x0002_QUITY UPLC I-Class system coupled to Waters VionTM IMS-QTOF_x0002_MS with high definition MSE data acquisition using the Wa_x0002_ters UNIFI software (Waters Corporation, Milford, MA, USA). An AccucoreTM VanquishTM C18+UHPLC (100 x 2.1 mm; 1.5 m parti_x0002_cle size) column (Thermo Fisher Scientific, Waltham, MA, USA) was used for chromatographic separation. Mobile phase A consisted of ultrapure water and B of methanol, each containing 2 mM ammo_x0002_nium acetate. The initial conditions of 20% B were held for 0.5 min, followed by a linear increase to 60% B at 4.5 min and to 90% B at 11 min. This was maintained for 4 min before returning to the starting conditions and equilibrating for 3 min. The flow rate was set at 0.3 mL min-1, the column temperature at 50 C, and the injection volume was 5 L Classification of fragment ions and selection of fragmentation flags. We analyzed the 34 PFAS standards mixture by MS/MS mode using an Agilent 1200 SL with Agilent 6560 IM-QTOF. Milli-Q water containing ammonium acetate (5 mM) and acetonitrile was used as the mobile phase for LC. The PFASs were separated with a Zorbax Eclipse Plus C18 column (2.1 mm _x0004_ 100 mm, 1.8 mm, Agilent Technologies) and examined by Dual Agilent Jet Stream negative electrospray ionization (ESI) mode We selected the abundant fragment ions as fragmentation flags for non-target analysis. To select a wide range of fluoroalkyl chain lengths up to carbon number 16, the fragmentation flags of PFASs homolog were inputted by considering mass differences of 49.9968 Da (eCF2e) and 99.9936 Da (eCF2CF2e) The samples were analyzed by LC/IM-QTOF-MS in all ions MS/MS mode We used ion mobility spectrometry to search for molecular ions of fragmentation flags. solution dansyl chloride (DNS-Cl) derivatization LC/MS/MS was investigated na total oxidizable precursor assay EPA Method 537.1 was applied to quantify PFASs (Shoemaker and Tettenhorst, 2018). Data independent IMS-MS-MS acquisition with support of ion mobility mass spectrometry (IMS) to distinguish the relevan ions from co-eluting ions HPLC-MSMS The extracts were analyzed using different LC-MS/MS methods for specific classes of analytes. Separation of short-chain PFCAs (C2eC4) was achieved using an ion-exchange RSpak JJ-50 2D column (2.0 mm i.d. _x0001_ 150 mm length, 5 mm; Shodex, Japan) (Taniyasu et al., 2008). For PFCAs (C4eC12), PFSAs, and diPAPs, an X-terra MS C18 column (2.1 mm i.d. _x0001_ 150 mm, 5 mm LC-MSMS TOPA The isotopic composition of biota samples (C and N) was eval_x0002_uated on defatted samples Combustion ion chromatography (CIC), The prevailing assumption has been that all PFASs are incinerated in CIC and matrix components have no impact on this process GC-MS equipped with a SUPELCOWAX column (60 m, 0.25 mm inner diam_x0002_eter, 0.25 m film; ultra-high pressure liquid chromatography-laminar flow tandem mass spectrometry (UHPLC-MS/MS) UHPLC-HRMS (UPLC-QToF continuous precursor/product ion mon_x0002_itoring mode identify unknown PFCs using experimental fragmentation patterns, mass defect filtering and Kendrick plots 2.1 mm x 100 mm Acquity HSS T3 1.8 m column held at 40 C with a 100 L injection loop Data processing of available datasets quantitative determination of extractable organically bound fluorine (EOF) solid-phase extraction (SPE) for extraction of fluorinated compounds as well as separation of interfering inorganic fluoride in combination with high-resolution-continuum source graphite furnace molecular absorption spectrometry combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) Extractable (EOF) and adsorbable (AOF) organically bound fluorine as well as total fluorine (TF) were measured na LC/(-)ESI-MS/MS Total fluorine (TF), extractable organic fluorine (EOF) by combustion ion chromatography (CIC) and poly- and perfluorinated compounds (PFCs) by LC-MSMS were measured a molecularly imprinted near-infrared excitation ratiometric fluorescent probe selectively recognition of specific cavities in the probe surface with analyte, accompanied by fluorescence quenching due to the photoinduced electron transfer effect between upconversion materials and PFOS UPLC system (Acquity H-Class with FTN injector; Waters, Milford, MA, USA) coupled to a Time-of-Flight mass spectrometer (QToF) (Xevo G2-S, Waters, Micromass; Manchester, UK) The LC separation was performed using an Acquity UPLC BEH-C18 column (Waters, 2.1 100 mm, 1.7 m particle size) for analyses in negative ionization mode and an Acquity UPLC HSS T3-C18 column (Waters, 2.1*100 mm, 1.8 m particle size) for anal_x0002_yses in positive ionization mode. The mobile phases used in positive ionization mode were (A): ultrapure water with 5 mM ammonium for_x0002_mate and 0.01% formic acid, and (B): acetonitrile with 0.01% formic acid. The mobile phases used in negative ionization mode were (A): ultra_x0002_pure water with 5 mM ammonium acetate with 0.01% ammonium hy_x0002_droxide and (B): acetonitrile with 0.01% ammonium hydroxide. The same gradient was used in both ion modes, and the flow rate was 0.5 mL min-1 . The gradient, expressed as %B, was 0.0 min: 5%B, 0.5 min: 5%B, 16.0 min: 95%B, 16.1 min: 99%B, 19.0 min: 99%B, 19.1 min: 5%B, and 21.0 min: 5%B. The injection volume was 5 L for all injections LC-MSMS CIC n automated, robust, cost-efficient and rapid CIC cryogenic air sampler (CAS), which was used to collect all atmospheric components simultaneously. Then, non-target analysis was performed through PFASs homologue analysis. UPLC-orbitrap Processed extracts were analyzed using an Agilent 1290 Infinity ultrahigh performance liquid chromatography (UHPLC) coupled to an Agilent 6530 Quadrupole Time-of-Flight HRMS (Santa Clara, CA, USA) with electrospray ionization in both positive and negative modes (ESI+/-), with full scan HRMS data acquired at the range of m/z 100-1700. For structure identification, MS/MS data was acquired (m/z 50-1700, collision-induced dissociation at 10, 20, and 40 eV) by datadependent acquisition using lists of preferred precursors based on initial MS-only screening. UHPLC separation used a reversed-phase C18 analytical column (Agilent ZORBAX Eclipse Plus 2.1100 mm, 1.8 m) with a C18 guard column (2.15 mm, 1.8 m). For ESI+, the mobile phase (0.4 mL/min) consisted of 5 mM ammonium acetate plus 0.1% acetic acid in each of water (A) and methanol (B) using a gradient of: 5% B at 0-1 min, 50% B at 4 min, 100% B at 17-20 min, 5% B at 20.1 min stop time 22.5 min; post-time 2 min. For ESI-, the mobile phase consisted of 1 mM ammonium fluoride in water (A) and methanol (B),31 using the same gradient. MassHunter Profinder (B.08.00) for non-target feature the adsorbable organic fluorine (AOF) method was improved and validated in this study Combustion and IC Analysis. Individual PFASs were quantified using liquid chromatography with tandem mass spectrometry (LC-MS/MS) and offline SPE Identification of potential contaminants was based on mass accuracy, isotopic ratio pattern, theoretical fragmentation, and retention time using Waters UNIFI software. The chromatography column and mobile phases were selected based on a pre-established screening method (Masi et al., 2013). The chromatograph was a Waters Acquity UPLC system (Milford, MA, USA). Chromatographic separation was carried out using a column Luna C18 (15.0 cm 0.21 cm) with a 3 m particle size (Phenomenex, Torrance, USA). A binary mobile phase of A (10 mM formic acid in water) and B (10 mM formic acid in methanol) was applied with follow_x0002_ing program: 0-15 min, 10% B; 15-18.5 min 95% B; 18.5-19 min, 95% B; 19-23 min, 10% B. The analytical column and the sample manager were kept at 35 C and 7 C, respectively. An aliquot of 10 L was injected into UPLC-QTOF-MS with a flow rate of 0.4 mL min-1 . A Xevo G2-S Q-TOF mass spectrometer (Waters, Milford, MA USA) was used in positive ESI na ninety-nine (99) PFASs and analysis of extractable organic fluorine (EOF) PFASs were analyzed using liquid-, supercritical fluid-, and gas chromatography coupled to mass spectrometry. EOF was analyzed using combustion ion chromatography. LC-MSMS ACQUITY BEH C18 column (2.1 50 mm; 1.7 m, Waters, USA) The mobile phase solvent gradient started at 65% of 0.1% formic acid in water, changed to 100% of 0.1% formic acid in ACN in 3.4 min, and returned to 65% of 0.1% formic acid in water at 4.7 min. The flow rate was set at 450 L/min with an injection volume of 6 L Extracts were analysed by HPLC-MS/MS using an Agilent Tech_x0002_nologies 1260 Infinity HPLC and an Agilent Technologies 6430 se_x0002_ries triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode. Adequate separation was ob_x0002_tained at a flow rate of 0.2 mL/min with a solvent gradient starting at 80:20 H2O/acetonitrile (v/v) reducing to 35:65 H2O/acetonitrile (v/v) at 15 min which returned to 80:20 H2O/acetonitrile (v/v) at 15.1 min, where it remained until the end of the run at 19.5 min LC-MSMS Phenomonex Luna Omega 2.1 50 mm, 1.6 m C18 column. Mobile phases consisted of ultra-pure water (A) and methanol (B), each with 2 mM ammo_x0002_nium acetate. Initial conditions of 20% B were held for 0.2 min be_x0002_fore being raised to 70% at 2.4 min, then 95% at 5 min. The gradient was then held at 95% for 2 min before returning to the initial con_x0002_ditions and equilibrated for 4 min. A flow rate of 0.6 mL min-1 and column temperature of 50 C were used throughout the run. An injection volume of 5 L was used. directly injecting 900 L of sample into a liquid chromatograph coupled to a triple quadrupole mass analyser, which involves minimal sample treatment as the sample only needs to be filtered Poroshell 120 EC-C18 (3 100 mm 2.7 m) equipped with a Poroshell 120 EC-C18 (3 5 mm 2.7 m) guard cartridge kept at 40 C. The mobile phase consisted of (A) water with 5 mM am_x0002_monium acetate and (B) MeOH. The elution gradient conditions were as follows: 2% B maintained for 4 min, increased to 40% over 2 min, increased to 90% over 9 min, after which 100% B was main_x0002_tained for 5 min and returned to initial conditions over 0.5 min and held for 3 min LC-MS/MS total fluorine (using particle-induced gamma ray emission) The Shimadzu LC system was coupled to a 5500 QTrap mass spectrometer , a SIL-30AC autosampler equipped with a 100 L loop, A delay column (C18, 100 x 4.6 mm) was installed between the mixer and the sample injector, in order to separate the impurity PFAAs originating from the LC system from the analyte PFAAs of the sample. ACQUITY UPLC BEH C18 column (100 x 2.1 mm, particle size 1.7 m) equipped with a guard column (Waters, Milford, MA, USA), thermostatted at 50 C, employing a mixture of 95% water 5% methanol solution of 2 mM ammonium acetate (solvent A) and a methanol solution of 2 mM ammonium acetate (solvent B) at a flow rate of 0.5 mL min-1. The chromatographic gradient was the following: 25% B for 2 min, from 25% to 90% in 6 min, 90% for 5 min, from 100% to 25% in 0.5 min and final hold for 6.5 min for system re-equilibration. Total analysis time was 20 mins. The injection volume used was set to 100 L UHPLC-MS/MS a Waters Acquity BEH C18 column (1.7 m, 2.1 mm 100 mm). 2 mM ammonium acetate aqueous solution (A) and acetonitrile (B) were used as mobile phases. The flow rate was 0.2 mL/min. The dualistic gradient started at 10% B, changed to 40% B in 3.5 min linearly, to 95% B in 5.5 min linearly; remained constant for 2 min; returned to 10% B in 0.5 min and then equilibrated for 3.5 min. The column oven was kept at 40 C and the auto-sampler was maintained at 10 C. An Agilent 1260 series RPLC was used to perform chromatographic analyses. The analytical separation was achieved using an Agilent Poroshell 120EC-C18 (3.0 50 mm, 2.7 m) column maintained at 30 C. A delay column (Agilent Eclipse Plus C18, 4.6 50 mm, 5.0 m) was installed after the mixing valve of the binary pump. The second valve was switched at 4 min. For chromatographic elution, the mobile phase was composed of acetonitrile (ACN) and water with 0.05% formic acid, and the flow rate was 0.30 mL min-1 . The gradient elution profile was programmed as follows: 0-4 min, 5% ACN; 4-9 min, 5-60% ACN; 9-16 min, 60-100% ACN; and, 16-21 min, 100% ACN. A 9 min re-equilibration period was included before the next analysis, resulting in an overall method run time of 30 min 300 C drying gas temperature at 7 L min-1 ; 350 C sheath gas temperature at 7 L min-1 ; 310 kPa nebulizer pressure; and, 3.5 kV capillary voltage LC-MSMS Acquity UPLC BEH C18, 1.7 m, 2.1 mm, 100 mm (Waters, USA) analytical column. The mobile phase con_x0002_sisted of the following 9-min sequence of linear gradients fows of solvent B (methanol) balanced with solvent A (0, 2.5 or 5 mM ammonium acetate in water) at a fow rate of 0.6 mL min-1: 40-65% B over 0.5 min, 65-95% B over 5 min, isocratic 95% B for 3.5 min and fnally 95-40% B over 0.1 min. The injection volume was 2 L, and column temperature was 40 C. na Agilent Liquid Chromatograph Se_x0002_ries 1200SL (consisting of a binary HPLC pump, an online vacuum degasser, an automatic sampler ALS and a thermostatted column com_x0002_partment and a DAD detector) coupled to a Agilent 6430 MSD triple_x0002_quadrupole mass spectrometer Hypersil Gold Aq column (3 30 mm, particle size 1.9 m) 60 C. An isocratic elution with 50% Milli-Q water containing 0.1% of acetic acid and 50% acetonitrile was performed with a flow rate of 0.2 mL min-1 and injection volume 10 L, allowing the separation of compounds within 10 min. Chromatographic analysis was carried out using an Agilent 1290 Infinity HPLC system consisting of a vacuum degasser, an autosampler and a binary pump (Agilent Technologies, Santa Clara, CA) equipped with a C-18 analytical column (Agilent ZORBAX Eclipse Plus C18, 50 mm 4.6 mm, 1.8 m particle size). 20 L of the sample extract was injected in each run. Mobile phases A and B were mili-Q water and acetonitrile, both with 0.1% (v/v) formic acid. The chromatographic method held the initial mobile phase composition (10% B) constant for 3 min, followed by a linear gradient to 100% B up to 25 min and kept for 3 min at 100% B. After each run, a 10-min equilibration was performed with the initial mobile phase composition. The flow rate was 0.5 mL min-1 . The HPLC system was connected to an time-of flight mass spectrometer (Agilent 6220 accurate mass TOF, Agilent Technologies, Santa Clara, CA) equipped with an electrospray interface operated in positive or negative ionization mode Online SPE-UPLC/LC/MS/MS was performed using a Thermo Fisher Scientific TSQ-Quantiva triple quadrupole mass spectrome_x0002_ter (Waltham, MA) once the sampling loading onto the SPETC was completed, the flow direction was reversed, and ana_x0002_lytes eluted onto the analytical column by a gradient of 20 mM ammonium formate in deionized water containing 1% ammonium hydroxide and methanol containing 0.4% ammonium hydroxide ramped from 80:20 to 100% basic methanol over 6 min. The mo_x0002_bile phase composition was held at 100% basic methanol for an ad_x0002_ditional 3 min, after which the column was rinsed with 100% ace_x0002_tonitrile (for additional rinsing and conditioning with a neutral pH, aprotic solvent), neutral deionized water, then returned to initial conditions to equilibrate for the next run. After seven minutes of runtime, the SPETC cartridge was removed from the sample path_x0002_way and rinsed with methanol for 11 min before equilibrating back to initial conditions of 100% deionized water The quantitative determination of PFAS was done with high-performance liquid chromatography (HPLC) using an Agilent 1200 series HPLC (Agilent Technologies, Waldbronn, Germany) and an Agilent 6460 (Agilent Technologies, Santa Clara, CA, USA) triple quadrupole mass spectrometer equipped with a jet stream electrospray ion source na na na A KinetexTM 1.7 m XB-C18 100 column (100 2.1 mm,i.d.) (Phenomenex, CA, USA) was used The optimized mobile phase was ethanol/water (70:30, v/v), pH 7.0, performed in isocratic mode using a flow rate of 0.20 mL min-1 using an eco-friendly solvent (ethanol) for both SPE procedure and UHPLC analysis, . Column oven and autosampler temperatures were set respectively at 35 and 4 C, and the volume of injection was 5 L The nanoparticles respond selectively and sensitively to trace concentrations of perfluorooctane sulfonate (PFOS) through electrostatic interactions between PFOS and NCDs Different concentration of PFOS and certain amount of NCDs was added into 10-mL cuvette, then the solution was diluted into 10 mL using pH = 6.1 BR buffer and mixed thoroughly. The final NCDs concentration and PFOS concentration was 2.5 mgmL-1 and 0, 3, 9, 10, 30, 50, 70, 90, 100, 140, and 160 10-10 molL-1 for a standard plot preparation. After incubated in the room temperature for 10 min, the solutions were transferred into 1-mL quartz cu_x0002_vettes for fluorescence spectra recording at excitation wave_x0002_length of 370 nm The tissue-level distribution of PFOS and PFOA in the roots and stems sections were identified with DESI-MS DESI 2D stage and analyzed using a Waters Xevo G2-XS mass spectrometer (Milford, MA, USA) in negative ion mode To help explain the results of DESI-MS, the cell-level distribution of PFOS and PFOA in the root cross sections was identified with TEM-EDS fluorine was carried out using an energy dispersive X-ray spectrometer HPLC-MS/MS CIC CIC for TF and EOF HPLC-MSMS LC-MSMS The instrumental analysis was performed according to (Sharma et al., 2016) LC-MSMS ACQUITY UPLC BEH C18 column (1.7 m 130 , 50 2.1 mm, Waters). When operated in negative ionization mode, the mo_x0002_bile phases employed were (A) H2O 2.5 mM NH4F and (B) MeOH 2.5 mM NH4F Combustion ion chromatographic technique for trace fluorine analysis was used to assess the concentrations of known PFCs (e.g., PFOS, PFOA) and total fluorine (TF) in the blood of wild rats Concentrations of PFCs in the whole blood samples were ana_x0002_lyzed by using high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) (UPLC-ESI-MS/MS) C18 BEH column (2.1 mm 100 mm, 1.7 m) coupled to a XEVO TQ-S MS/MS instrument. The mobile phases were MeOH and a 30:70 MeOH/water mixture, both with 2 mmol/L ammonium acetate and 5 mmol/L 1methylpiperidine as additives, and the column was kept at 50 C. Ultra-short-chain compounds (C2-C3) were separated by a supercritical fluid chromatography system EOF: combustion ion chromatography (CIC); this method has been published by Yeung et al LC-MSMS TOP Indoor dust samples were oxidized with TOP assay optimized in our previous study GC-MS LC-MSMS UHPLC-Q-Orbitrap HRMS A full scan was firstly run and then a dd-MS/MS scan. All the target compounds were monitored within the 5 parts-per-million mass error range (5 ppm). ultrahigh performance liquid chromatography coupled to a high-resolution mass spectrometer (UHPLCHRMS) na Ultra high performance liquid chromatography system coupled with a Thermo ScientificTM Q-ExactiveTM Focus Orbitrap high resolution mass spectrometer nontarget high-performance liquid chromatography (HPLC)-Orbitrap Liquid chromatography-negative ion electrospray tandem mass spectrometry (LC-MS/MS) Liquid Chromatography-Mass Spectrometry Instrumentation Gas Chromatography-Mass Spectrometry Instrumentation TOP Assay Instrumentation: LC-MS AOF Instrumentation: modified combustion ion chromatography (CIC) system Ion exchange liquid chromatography coupled with negative-ion electrspray tandem mass spectrometry (IC-MS/MS) Triple Quadrupole LC/MS or LC-MS/MS according to ISO21675 (LC-MS/MS) 1) Method 537.1: Determination of Selected PFAS in Drinking Water by SPE and LC/MS/MS (2018/2020) ->Drinking (Potable) Water 2) Method 537: Determination of Selected PFAS in Drinking Water by SPE and LC/MS/MS (2009 - listed for historical purposes) ->Drinking (Potable) Water 3) Method 533: Determination of PFAS in Drinking Water by Isotope Dilution Anion Exchange SPE and LC/MS/MS (2019) -> Drinking (Potable) Water 4) MediaMethod Description -> Drinking (Potable) Water 5) Method 8327: PFAS Using External Standard Calibration and MRM LC/MS/MS (2019) -> Drinking (Potable) Water 6) Method 8327: PFAS Using External Standard Calibration and MRM LC/MS/MS (2019) -> Non-Potable Water and Other Environmental Media 7) Draft Method 1633 -> Non-Potable Water and Other Environmental Media 8) Other Test Method (OTM)-45 -> air emissions 9) SW-846 Test Method 0010: Modified Method 5 Sampling Train -> air emissions 10) Modified Method TO-15 -> air emissions 11) Ambient/Near-Source (coming soon) -> ambient air 12) Semivolatile PFAS (coming soon) -> ambient air 13) Volatile PFAS (coming soon) -> ambient air 14) Total Organic Fluorine (TOF) (coming soon) -> Total 15) Total Organic Precursors (TOP) (coming soon) -> Total NON-EPA 1) CLG - PFAS 2.03 Screening, Determination and Confirmation of PFAS by UPLC-MS-MS 2) Bottle Selection and other Sampling Considerations When Sampling for Perand Poly-Fluoroalkyl Substances (PFAS) 3) CDC - Laboratory Procedure Manual - 6304.09 - Online Solid Phase Extraction-High Performance Liquid ChromatographyTurbo Ion Spray-Tandem Mass Spectrometry (online SPE-HPLC-TISMS/MS) in serum 1) Draft method 1633 for 40 PFAS compounds 2) Draft method 1621 for adsorbable organic fluorine PFAS strategic roadmap learn about EPA actions and accomplishments since January 2021 LC-HRMS Quantification method Working range (ng/ mL) As Matrices Internal and external standards. If commercially available, the method analytes must be purchased as technical grade (linear and branched isomers) standards or neat materials. na Drinking water calibration uses a solution containing the analytes of interest and internal standards 2,0 ng/l to 10 000 ng/l for PFOS and 10 ng/l to 10 000 ng/l for PFOA Water external standard calibration working range of the LC/MS/MS system Non-potable water Calculate the concentration in the sample using the linear or quadratic calibration curve generated. 25-1000 ng/kg, except for PFOS, PFHxA(50-1000 ng/kg), PFPeA, PFBA (125-5000), FHEA (600-20 000), FOEA (750-20 000), FDEH (500-20 000) Soil Internal & external standard (at a 10 - 400 ng/L, 50 - minimum, five calibration levels are 2000 ng/L for PFPeA, Water required when using a linear PFBA, 200 - 8000 Sludge calibration curve and six calibration ng/L for FDEA, 300 - Influent levels are required when using a 8000 ng/L for FOEA, Effluent quadratic calibration curve.) FHEA Wastewater External and internal standards calibration from 10 Soil Sediment g/kg to 500 g/kg Sludge Internal standard quantitation, Isotope dilution (ID) quantitation na Water, Soil, Tissue Calibration Curves na Air Calibration using a external or internal standard The lower limit of application is 0,01 g/l, or 0,025 g/l for treated waste water. Water Internal or external Calibration uses PFAS were analysed a solution containing the native in five samples which analytes of interest and labelled were spiked with internal standards. Internal analytes within a standard calibration is preferred concentration range when the internal standards are of 0,55 ng/l to 200 available ng/l. Water Internal and external standards. If commercially available, the method analytes must be purchased as technical grade (linear and branched isomers) standards or neat materials. na Drinking water Isotope Dilution The user may modify the concentrations of the individual analytes based on the confirmed MRLs and the desired monitoring range. Drinking water na na surface water isotope surface water and aquatic na invertebrates na na water Marine mammal na na liver samples na na river water na na water na na water na na air na na water na qualitative na water na water precipitation na na samples water, sediments na na and biota surface water and whole-blood na na sample extracts na na na na na water Deciduous leaves, na na Grass na na fish na na na na na surface water na na water na na na na na na na na sediment water, serum and na na egg The target compounds were identified by UNIFI using accurate mass screening (maximum 10 ppm mass error) and retention time (1-min time window). UNIFI was also used to group all isotopes and adducts to_x0002_gether as one identified compound when processing the data,, na na na qualitative na water na air na na na na na water The workflow (Fig. 1) and identification confidence criteria used on suspect and non-target screening were based on those described by Krauss et al. (2010), Schymanski et al. (2015) and Pedersen et al. (2013). na na na water na bird eggs, fish, marine mammals, terrestrial mammals, surface water, WWTP effluents and na na sludge, and air na na feathers Quantification was achieved using a 9- point blank-offset and internal standard-corrected calibration na na isotope na na na water na na Dust and wipe na na na external standard and isotope dilution na fish na na na na na na na The internal standard concentration (Ketoprofen-d3) was maintained constant at 25 ng mL-1 , while the analyte concentra_x0002_tions were 2, 5, 10, 15 and 30 ng mL-1 . Each point of the respective cal_x0002_ibration curves was the mean of three replicates. All analytes showed good linearity (R2 between 0.992 and 0.999). na sediment urine and hair, airborne particles, tap water and bottled water na accurate mass database na na sotope dilution quantification na water internal standard calibration curves with eight concentration points na na na LC/ (-)ESI-MS/MS Water, sediment and biota na Surface, ground and drinking water water and human na na serum samples na na na na na water na na na isotope na na na na surface water na liver na water na mussel na na blood isotopically labeled IS na na na water na na na dust Quantification was performed via UHPLC-HRMS na suspended particulate matter (SPM) na na soil isotope dilution The linear ranges for target analytes were from 1 to 250 ng/g, with R2 values of 0.98 or higher, except for PFBS and 4:2 FTS, which were found to be linear from 5 to 250 ng/g with R2 values of 0.99 Waste-activated sludge (WAS) and limestabilized primary solids (PS) Legacy PFASs were quantified using authentic standards, and nontarget PFASs were semiquantified against structurally similar authentic standards na Fish (liver) Internal standard quantitation, Isotope dilution (ID) quantitation 19 different calibration curve commercially ranging in available composts, concentrations from garden soils, and 0.05 to 100 ng ml- 1 potting mixes Internal standard quantitation, Isotope dilution (ID) quantitation na 16 surface water samples, 16 bank filtrate samples, 7 raw water samples, and 7 groundwater samples Internal standard quantitation, Isotope dilution (ID) quantitation 0.02 - 10 g/L leaf samples internal standard method na biota (fruits and vegetables: blackberries, blueberries, corn kernels (corn), grapes, okra, peaches, pecans, potatoes, squash, and tomatoes) drinking water, river water sea water, and effluent of wastewater from a sewage treatment na na plant from Japan na na water, air, serum na na na na na na na na fish and serum Reported levels (ng/mL) Limitations LoD (ng/mL) subgroup Single laboratory LCMRLs (laboratory lowest concentration minimum reporting level) for analytes in this method range from 0.53-6.3 ng/L. Determining the Detection Limit (DL) for analytes in this na na method is optional. Considerable batch- to-batch differences in quality and selectivity of these materials are na possible. na Matrix interferences can be caused by contaminants from the sample, sampling devices, or na storage containers. na This test method was tested by CRL on Ottawa sand and ASTM reference soil. na LoQ: 0.01-0.25 g/kg RL: 0.25 g/kg This test method was tested by CRL on reagent water. na MDL (ng/L) = 0.7 (PFTriA) - 4.6 (PFBA, PFPeA), 47.2 (FDEA), 92.9 (FHEA), 106.8 (FOEA) na na LoQ: 10 g/kg na The LOQ shall be set at or above the concentration of the lowest initial calibration standard (the lowest calibration matrix interferences standard must fall for specific within the linear na compounds range). na na na na na na na na Substances with similar retention times that can produce ions with similar mass to charge ratios (m/z) to those produced by the analytes of interest may interfere with the determination. Matrix interferences may be caused by contaminants that 0,2 ng/l as limit of are coextracted quantification can be na from the samples. achieved na Single laboratory LCMRLs (laboratory lowest concentration minimum reporting level) for analytes in this method range from 0.53-6.3 ng/L. Determining the Detection Limit (DL) for analytes in this na na method is optional. Matrix interferences may be caused by contaminants that are co-extracted na from the sample. na na only 24%-63% of the EOF can be explained by targeted PFAS A distinct signature of AFFF contamination enriched in precursors with six perfluorinated carbons (C6) was identified in watersheds with an AFFF source, while others were enriched in C4 precursors. Principal component analysis of PFAS composition in impacted watersheds showed a decline in precursor composition relative to AFFF stocks and a corresponding increase in terminal perfluoroalkyl sulfonates with < C6 but not those with C6 na .005 to 2.62 ng L-1 na S25PFASs concentration in water was 1920 ng L_x0001_1 high amounts of EOF (e.g. 8.2 g F day_x0001_1 at site A) could be transported by water to recipient water bodies relative to S25PFASs (e.g. 0.15 g day_x0001_1 at site A). na emerging PFASs, 24 were detected, with a sum ranging from 2.7 ng/L (Alz River) to 420,000 ng/L (Xiaoqing River). the increase of the short-chain compound PFBA was higher in German samples than in Chinese samples (88 30% versus 12 14%) na 7:3 FTCA in polar bears (~1000 ng/g, ww) and cetaceans (<6-190 ng/g, ww) 30-75% of 15 the EOF was unidentified. Suspect screening revealed an additional 37 PFASs (not included in the targeted analysis) bringing the total to 63 detected PFASs from 12 different classes na na na 0.004 and 0.81 ng L_x0001_1 for water samples and between 0.03 and 0.37 ng g_x0001_1 for aquatic invertebrate 16 ng F ranged from 257-782 ng F L_x0001_1 in the neutral fraction and 71-217 ng F L_x0001_1 in the anionic fraction na 0.017 ng/L (FOSA) to 0.33 ng/L (PFBA) MQLs were in the range of 0.50 ng/L (PFUnDA) to 2.5 ng/L (PFOS) for unoxidized samples and of 0.50 ng/ L (PFUnDA) to 7.9 ng/L (PFOA) for oxidized samples na na na 0,1 mg/L SPE: 0,3 g/L na f 3-7 compounds from the targeted list and the detection of a further 56-107 untargeted PFAS The measured concentrations ranged from 2.9 1.5 to 257.3 11.2 ng L-1 na between 0.19 and 0.76 g L-1 na na na D (10 : 2 FTOH) to 300 pg m(-3 )(6 : 2 FTOH) na SPFAS concentration was observed at the point-source (mean 5500 ng/L; 95% CI: 4800, 6300) relative to upstream sites (mean 100 ng/L; 95% CI: 90, 110; p _x0002_ 0.001). The point-source SPFAS concentration decreased from 5500 1200 ng/L to 960 42 ng/L (_x0003_83%) after two months and to 430 15 ng/L (_x0003_98%) two years later. na na na 1.5 pg m(-3) (6 : 2 FTOH) to 9.9 pg m(-3) (4 : 2 FTOH) na na na 13 PFASs were detected in source and drinking water with total concentration of 25-38 ng/L mass flow in the wet season (i.e. summer) up to 83 kg/d. na suspect screening of PFASs with eternal database resulted in de_x0002_termining 32-96 PFAS suspects in firefighting foam impacted groundwater samples na TFA displayed the highest concentrations (8.8-1.8x 103 ng/L) 6:2 chlorinated polyfluorinated ether sulfonic acid, an alternative to PFOS, was detected for the first time in precipitation at a frequency of 43% (C4eC12; 2.0 _x0001_ 102 e3.4 _x0001_ 103 ng/m2 /d) with major PFAS manufacturing facilities were higher than those in the southwestern area (63e1.7 _x0001_ 103 ng/ m2 /d pre-PFAAs at 3.1 _x0001_ 103 and 4.3 _x0001_ 103 ng/m2 /d na (2.0-147 ng g_x0001_1 wet weight), perfluorooctane sulfonate (PFOS) and C12-C14 perfluoroalkyl carboxylates (PFCAs) being predominant while Ppre- PFAAstargeted contributed to 1-18% of PPFASs Trophic magnification factors (TMFs) were >1 na na na na na na na 0.003-0.34 ng L_x0001_1 , 0.014-0.35 ng g_x0001_1 dw and 0.005-0.21 ng g_x0001_1 wet weight (ww) na na na 65-223 pg m-3 for fluorotelomer alcohols (6FTOHs); 1.2-12.8 pg m-3 for fluorinated sulfonamides (6FOSA); and 0.29-1.02 pg m-3 for fluorinated sulfonamidoethanols (6FOSE) na 50 ng/mL na na na d LOQs of 2.5 ng L- 1 (PFOS) and 1 ng L - 1 (GenX, na na PFBS and PFOA) na 4.3-86 ng/g (n = 5), 1.0-27 ng/g (n = 5) linear perfluoroalkyl carboxylic acids (C4 to C14) and perfluoroalkyl sulfonates (C4, C6, C8 and C10) exhibited a linear range spanning over three orders of magnitude na perfluorooctane sulfonate (PFOS) was often a dominant PFAS in a given surface water sample, frequently followed by perfluorohexane sulfonate (PFHxS). Second, that a four_x0002_chemical mixture generally accounted for > 80% of the sum of all routinely-reported PFAS in a sample and that the most representative four chemical mixture was comprised of PFOS, PFHxS, perfluorohexanoic acid (PFHxA) and perfluorooctanoic acid (PFOA) na 50-300 ng/L na TF concentrations determined via HR-CS-GFMAS and CIC were comparable between 148 and 270 g/ L. AOF making up 0.14-0.81% of TF (determined using CIC) and EOF 0.04-0.28% of TF (determined using HR-CS-GFMAS) na less than 1 pg on column 0.01 - 0.11 ng/g na na na low nanogram per liter range na na na na na na na na na na na total concentrations of PFCs (PPFCs) reached a maximum in the later 1990s and early 2000s na na na na na 1 pmol/L na 7,5 ng/L na na na surface water varied between 2.3 and 24.5 g/L. The concentrations of AOF in 85% of the wastewater discharges were be_x0002_tween 2.0 and 8.5 g/L, while 15% of the samples were below the limit of quantitation (LOQ = 2 g/L AOF). In 56% of the ground water samples the values were below the LOQ. In 44% of the surface water samples (n = 41) the values were between 2.0 and 6.1 g/L AOF 14 individual PFAS were determined by LC-MS/MS. AOF values up to 555 g/L na na na A total of 117 PFAS homologues (38 classes) were discovered, 48 of which (13 classes) were identified with confidence level 4 or above na na na (PFOS) concentrations were as high as 72-140 ng/L na the TF concentration of FireAde (4.3 g/L) is about 1.6 times and 3.5 times higher than EOF and AOF concentrations, respectively. Similarly, T-Storm contains 4.4 g/L of TF, about 2.3 and 4.0 times higher than EOF and AOF concentrations, respectively. Meanwhile, in the Buckeye sample, EOF concentration (10 g/ L) is slightly higher than TF (9.1 g/L), and AOF (4.8 g/ L) after TOP assay treatment, 11 PFCAs (C4-C14) were detected at the levels of 8-399 mg/L na na na 300 and 400 ng/L AOF analysis are conservatively defined based on 1 mg/L na na na na na The range of total PFAS concentrations in egg samples were 627 - 707 ng/g w.w. for Sweden, 44.9 - 99.9 ng/g w.w. for Iceland, and 56.9 - 81.4 ng/g w.w. for Faroe Islands. Among the marine mammals, polar bear liver samples (Ursus maritimus) from Greenland showed the highest sum of PFASs (1426 - 1890 ng/g) as well as highest EOF (1782 - 2056 ng fluoride/g). The total PFASs in other marine mammal samples ranged between 35.1 ng/g in grey seal (Halichoerus grypus) from Denmark to 123 ng/g in harbour porpoise (Phocoena phocoena), also from Denmark. The PFASs in surface water mainly ranged between 1 and 10 ng/L The target analysis of PFASs could explain between 2% and 102% of the measured EOF na na na na na 30-126 ng F/L EOF na na na na na Levels of perfluorinated compounds (PFCs) perfluorooctanoic acid (PFOA) and perfluorononanoic acid (PFNA) maximum levels of 1160 ng/L, 647 ng/L and 2405 ng/L na 0,23-1,52 ng/L na below the limit of quantification to 898 15 ng L-1 na na na The highest _x0002_PFASs level found in a sample was 32.0 ngL-1 in influent The sum of the mean concentrations of the target PFASs determined in the influ_x0002_ent (8.6 ngL-1) and the effluent (8.2 ngL-1) are very close na between 0.1 and 2.0 ngL-1 na The 24 PFAS accounted for less than 2% of fluorine in dust (n = 39), suggesting the potential presence of unknown PFAS. The median total fluorine concentration in sampled fire station rooms was 157 g/g PFAS: 60-189 ng/g na TF detection limit (MDL) was 25 g/g na na na 0.014-0.44 ng L-1 na 9PFASs con_x0002_centration range of 0.04 to 2.14 ng/g wet weight na 2 pg/g to 10 pg/g na na na 0.16 to 5.13 ng L-1 na na na All target PFASs were detected in at least 32% of urine samples, with geometric mean (GM) concentrations ranging from 0.18 to 2.97 ng/L, and in 100% of drinking water samples at GM concentrations of 0.18-21.1 ng/L. 48-70% of hair samples (GM concentrations: 2.40- 233 pg/g) and 100% of air samples (GM concentrations: 14.8-536.7 pg/m(3)). na Mar-13 na 0.090 to 3.7 pg g-1 dry weight na na na limit of detection of 0.15 ng mL-1 and a limit of quan_x0002_titation of 0.50 ng mL-1 . Nonetheless, for practical reasons, the lowest point of the calibration curve (2 ng mL-1 ) was considered as the limit of quantitation for all of the compounds. na na na na na na na Mean PFAS concentration in the landfill leachate was 643 84 ng L-1, while it was 365 8.0 ng L-1 in a freshwater pond and 57 4.0 ng L-1 in a creek in the vicinity of the FFTS. These levels were an order of magnitude higher than in coastal seawater of the nearby fjord (maximum level PFAS = 10.1 1.2 ng L-1, at the FFTS impacted site). PFOS was the most predominant compound in all seawater samples and in freshly fallen snow (63-93% of PFAS). In freshwater samples from the Longyear river and the reference site, PFCA C9 were the predominant PFAS (37-59%), indicating that both local point sources and diffuse sources contributed to the exposure of the marine food web in the fjord. PFAS concentrations increased from zooplankton (1.1 0.32 g kg-1 ww) to polychaete (2.8 0.80 g kg-1 ww), crab (2.9 0.70 g kg-1 ww whole-body), fish liver (5.4 0.87 g kg-1 ww), and gull liver (62.2 11.2 g kg-1). na 1,4-5,9 ng/L na na na sub ng/L to single digit ng/L na in ng/g Water: 0.03 - 1.08 for different coumpounds Fish: 0.0.1 - 0.0.9 Sediment: 0.01 - 2 Crab: 0.01 - 1.11 Plankton: 0.002 - 8.82 Worms: 0.01 - 5.3 na LOQ: 0,55-3,20 ng/L na 0.1-3.3 ng/L ). The detection limit (LOD) calculated from 3/K na na to be 0.1 ng L-1 na na na na na na 0.3 nM na na na targeted: 0.43 to 519 ng/L IF was the major contributor to TF in water samples na PFOS was the dominant PFC in the tissues at concentrations ranging at 26-693 ng/g ww in dolphins and 51.3- 262 ng/g ww in porpoises a large proportion (w70%) of the organic fluorine in both species is of unknown origin na na na t organic pollutants were not detected in any sample na na na e 0.03 ng/L for seawater and lake water, 0.10 ng/L for snow, and 2 ng/L for runoff water na na na na na < 30 ng/g na PFCs (PFOS, PFOSA, PFUnDA, PFDA, PFNA, and PFOA) were detected in all of the wild rat blood samples. Con_x0002_centrations of extractable organic fluorine (EOF) in fraction 1 (Fr1; MTBE extraction) of wild rats ranged 60.9-134 ng F mL-1, while those in fraction 2 (Fr2; hexane) were below LOQ (32 ng F mL-1); TF concen_x0002_trations in the blood of wild rats ranged from 59.9-192 ng F mL-1. The contribution of known PFCs in EOF-Fr1 (MTBE) varied from 9% to 89% (56% on average), and known PFC concentrations in TF content were less than 25%. In contrast, TF concentrations in the blood of PFOA-exposed rats ranged from 46900 to 111000 ng F mL-1, with PFOA contributing over 90% of TF na na na on average 90% of the EOF could not be explained by the 73 PFAS monitored EOF. in effluent (324-1460 ng of F/L) and sludge (39-210 ng of F/g of dry weight) na field log Kd of 1.3-2.2, With total oxidizable precursor assay, unknown precursors for C2-C3 perfluoroalkyl carboxylic acids (PFCAs) (57-99 mol%) contributed more than those for C4-C12 PFCAs in the three mediums na EOF: 560 ng of F/g; na na na PFASs in outdoor dust tripled from 63 to 164 ng/g In 2017, the indoor dust levels of PFASs were in the range 185-913 ng/g, which were generally higher than the outdoor dust levels (105-321 ng/g). Emerging PFASs were found at high median levels of 5.7-97 ng/g in both indoor and outdoor dust samples unknown perfluoroalkyl acid (PFAA)- precursors contributed 37-67 mol % daily perfluorooctanoic acid (PFOA) equivalent intakes of PFAAs (C4- C12) mixtures via indoor dust were first estimated at 1.3-1.5 ng/kg b.w./d for toddlers na Twenty PFASs were detected with the total concentration of 0.3-32.9 ng/L, indicating the contamination level similar to that in drinking water. The dominant PFASs were perfluorobutanesulfonate (PFBS), perfluorobutanoic acid (PFBA), perfluoropentanoic acid (PFPeA) and perfluorooctanoic acid (PFOA) na na excellent method limits of quantification (MLOQs) (0.5-250 pg/ L), Target analysis detected total PFAS concentrations (PFAStarget) in SPM in the range of 0.336-14.9 g kg-1. PFAS concentrations determined by dTOP assay (PFASdTOP) were considerably higher than those found by target analysis (i.e.,PFASdTOP: 5.55-331 g kg-1 the different sorption properties of various PFAS may introduce a bias in the temporal evaluation and the results cannot be extrapolated to the water phase. The LOQs were 0.05-0.5 g kg-1 dw for target analysis and 1.0 g kg-1 dw for the dTOP assay It is known that high levels of organic matter in biosolid samples interfere with the oxidation process and lead to an incomplete transformation of na precursors na concentrations of individual PFAS (27 targeted analytes) can range from 0.6 to 84.6 ng/g in WAS (average total PFAS = 241.4 ng/g) and from 1.6 to 33.8 ng/g in PS (average total PFAS = 72.1 ng/g) na PFCAs were generally present at very low levels in all fish (i.e., PFCAs < 46 ng/g). The Tangxun lake fish generally had higher levels of PFSAs than the Yangtze River fish (i.e., PFSAs: 50-950 versus 7-25 ng/g, respectively) na The total (38) PFAS in the samples ranged between 1.26 to 11.84 g kg- 1 (dry weight) na LOD: 0.5 - 7.7 ng/g LOQ: 1.5 - 25.7 ng/g LOQ: 0.02 - 2.1 ng/g in wet liver (instrumental LOD) 0.012 - 2.5 ng/mL DWD PFAS (18/20): 0.0003 - 0.0772 g/L ultra-short-chain PFAS: 0.0005 - 12.41 g/L Ultrashort-chain PFASs, however, remain a blind spot even for these "PFAS total" parameters 0.0000625 - 0.1 ng/mL (method LOQ for GC and LC) The highest concentrations (up to 1000 g/kg dry weight) were found in Lombardy poplar (Populus nigra `Italica') leave na 18 - 30 g/kg dw (LOQ) The MQLs (method quantification limits) of 45 PFAS (including 13 PFEAs) in 10 matrices ranged from na na 0.025 to 0.25 ng/g na several difficulties were noticed in measureing PFAS in seawater, greater amounts of adsorbent are necessary and removal of non- volatile salts. Novel techniques (in-situ SPE and purge and trap extraction) were evaluated and The six water samples (drinking water, river water, further seawater, and development, wastewater) showed concentration ranges of 0.55 optimization, and ng/L to 200 ng/L for validation are samples A through E, and 8000 ng/L for Sample F needed. na na na na na na na na na na na na na na na na na na Measurement - generic name LC-MS/MS LC-HRMS LC-MS/MS HR-CS-GFMAS CIC, HR-CS-GFMAS LC-MS/MS CIC, LC-MS/MS LC-MS/MS LC-MS/MS, CIC LC-HRMS LC-MS/MS CIC, LC-MS/MS LC-MS/MS CIC LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS DESI-MS LC-MS/MS LC-MS/MS CIC, LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS LC-MS/MS, TOP assay TOP assay, GC-MS, LC-MS/MS LC-HRMS LC-MS/MS LC-HRMS LC-HRMS LC-MS/MS TOP assay, LC-MS/MS, CIC IC-MS/MS LC-MS/MS LC-MS/MS LC-HRMS Title Authors EPA method 533 for PFAS analysis in drinking water at low parts-per-trillion levels Butt et al. Analysis of Per/Polyfluoroalkyl Substances in Water Using an Agilent 6470 Triple Quadrupole LC/MS Hunt et al. AOF by combustion IC - non-targeted complemental determination of PFAS in aqueous samples von Abercron et al. Direct analysis of selected per- and polyfluorinated alkyl substances (PFAS) in ground, surface, and waste water by LC-MS/MS Jacob et al. Extraction and analysis of poly- and perfluoroalkyl substances (PFAS) from soil MacLennan et al. Direct Injection Analysis of Organofluorine Compounds (PFAS) by Triple-Quadrupole LC/MS/MS na Rapid LC-MS/MS method for monitoring bio-relevant levels of perand polyfluoroalkyl substances (PFAS) in serum Negri et al. Analysis of EPA Method 537 per- and polyfluoroalkyl substances (PFASs) using microflow liquid chromatography Oetjen et al. Analysis of legacy and emerging perfluorinated alkyl substances (PFAS) in environmental water samples using solid phase extraction (SPE) and LC-MS/MS Organtini et al. Large volume direct injection method for the anaysis of perfluorinated alkyl substances (PFAS) in environmetal water samples in accordance with ASTM 7979-17 Organtini et al. A method for the extraction and analysis of PFAS from human serum utilizing weak anion exchange (WAX) chemistry and Xevo TQ-S micro Organtini et al. Analysis of Per/Polyfluoroalkyl Substances (PFAS) in Drinking Water by EPA 537.1 and EPA 533 Using the Agilent Ultivo Triple Quadrupole LC/MS Pierri et al. Analysis of PFAS in Drinking Water with EPA Method 537.1 and the SCIEX QTRAP 4500 System Roberts et al. Analyses of PFOS and PFOA Precursors in Textile Products Using EI-MRM and PCI-SIM Method Yeong et al. Determination of per- and polyfluorinated alkyl substances (PFAS) in drinking water Zhang et al. Detection and treatment strategies of per- and polyfluoroalkyl substances (PFAS): Fate of PFAS through DPSIR framework analysis John et al. Journal year Sciex application note 2021 Agilent application notes 2017 Thermo application notes 2020 Thermo application notes 2019 Thermo application notes 2021 Shimadzu application note 2020 Sciex application note 2020 Sciex application note 2020 Waters application notes 2020 Waters application notes 2020 Waters application notes Agilent application notes 2021 2020 Sciex application note 2019 Shimadzu application note 2018 Thermo application notes 2020 Journal of Water process engineering 2021 comments na DOI link na na na na na na na na na na na na na na na na na na na na na na na na na na na na na REVIEW - In this comprehensive review, a Driver-Pressure-State-Impact-Response (DPSIR) framework has been proposed to understand PFAS from the source of emission and their impacts on the environment. DPSIR framework is a conceptual model used to describe, analyze, and understand environmental problems. Different treatment strategies for the removal of PFAS are discussed in this review. https://www.sciencedirect.com/scienc Name PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, 4:2 FTS, 6:2 FTS, 8:2 FTS, PFMPA, PFMBA, HFPO-DA, NFDHA, PFEESA, DONA, 9Cl-PF3ONS, 11Cl-PF3OUS PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA, PFTeDA, FOSA, N-EtFOSAA, N-MetFOSAA, FHEA, FOEA, FDEA, PFHpPA, 4-2 FTS, 6-2 FTS, 8-2 FTS, 6-2 FTUA, 8-2 FTUA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS TFA, PFPA, PFBA, PFPeA< PFHxA, PFHpA, PFOA, PFNA, PFDA, TMSA, PFBS, PFHxS, PFOS, H4PFOS, Chiron AS, PFPS, PFPrS, HFPO-DA, PBSF, POSF, 4-FBA PFBS, PFHXS< PFOS, 4:2 FTS, 8:2 FTS, PFPeS, PFHpS, PFNS, PFDS, PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUdA, PFDoA, PFTrDA, PFTeDA, NEtFOSAA, NMeFOSAA, FOSA, M3PFHxS, M8PFOS, M4PFBA, M5PFPeA, M5PFHxA, M4PFHpA, M8PFOA, M9PFNA, M6PFDA, M7PFUnA, MPFDoA PFBA, C4-PFBA, PFPeA, C6-PFPeA, PFBS, C3-PFBS, PFMBA, PFEESA, NFDHA, C6PFHxA, 4:2FTS, C2 4:2 FTS, PFHxA, C5PFHxA, PFPeS, C3-PFHxS, HFPO-DA, C3-HFPO-DA, PFHpA, C4-PFHpA, PFHxS, ADONA, 6:2FTS, C2-6:2FTS, PFOA, C8PFOA, PFHpS, PFNA, C9-PFNA, PFOS, C8-PFOS, 9Cl-PF3ONS, 8:2FTS, C2-8:2FTS, PFDA, C6-PFDA, PFUnA, C7-PFUnA, 11ClPF3OUdS, PFDoA, C2-PFDoA PFOA, PFOS, 4:2 FTS, 6:2 FTS, 8:2 FTS, 10:2 FTS, N-EtFOSA, N-EtFOSAA, N-EtFOSE, FOSA, N-MeFOSAA, N-MeFOSE, NMeFOSA, PFTrDA, PFBA, PFBS, PFDA, PFDoDA, PFHpA, PFHxA, PFHxS, PFPeS, PFNA, PFOA, PFDS, PFHpS, PFOS, PFPeA, PFTeDA, PFUnDA, PFHxDA PFBS, PFPeA, PFHxA, PFPeS, PFHpA, PFHxS, PFOA, PFHpS, PFNA, FOSA, PFOS, PFDA, PFNS, PFUdA, PFDS, PFDoA, PFTrDA, PFTeDA. PFHxDA, PFODA, PFDoS na PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTriDA, PFTreDA, PFHxDA, PFODA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, N-MeFOSAA, N-EtFOSAA, FHUEA, FOUEA, 8_2 diPAP, 4_2 FTS, 6_2 FTS, 8_2 FTS, PFecHS, FHEA, FOEA, FDEA, FHpPA, ADONA, Cl-PF3ONS, 11Cl-PF3OUdS, GenX, PFMBA, NFDHA, PFEESA, 13C-PFBA, 13C5-PFPeA, 13C5-PFHxA, 13C4-PFHpA, 13C8-PFOA, 13C9PFNA, 13C6-PFDA, 13C7-PFUnDA, 13C-PFDoDA, 13CPFDoDA, 13C2-PFTreDA, 13C2-PFHxDA, 13C3-PFBS, 13C3PFHxS, 13C8-PFOS, D5-N-EtFOSAA, D3-N-MeFOSAA, 13CFOUEA, 13C4-8:2 diPAP, 13C2-4:2 FTS, 13C2-6:2 FTS, 13C28:2 FTS, 13C-FHEA, 13C-FOEA, 13C-FDEA, 13C3-GenX PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTriDA, PFTreDA, PFHxDA, PFODA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, N-MeFOSAA, N-EtFOSAA, FHUEA, FOUEA, 8_2 diPAP, 4_2 FTS, 6_2 FTS, 8_2 FTS, PFecHS, FHEA, FOEA, FDEA, FHpPA, ADONA, Cl-PF3ONS, 11Cl-PF3OUdS, GenX, PFMBA, NFDHA, PFEESA, 13C-PFBA, 13C5-PFPeA, 13C5-PFHxA, 13C4-PFHpA, 13C8-PFOA, 13C9PFNA, 13C6-PFDA, 13C7-PFUnDA, 13C-PFDoDA, 13CPFDoDA, 13C2-PFTreDA, 13C2-PFHxDA, 13C3-PFBS, 13C3PFHxS, 13C8-PFOS, D5-N-EtFOSAA, D3-N-MeFOSAA, 13CFOUEA, 13C4-8:2 diPAP, 13C2-4:2 FTS, 13C2-6:2 FTS, 13C28:2 FTS, 13C-FHEA, 13C-FOEA, 13C-FDEA, 13C3-GenX PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTriDA, PFTreDA, PFBS, PFPeS, PFHxS, PFHpS, PFOS, PFNS, PFDS, FBSA, FHxSA, FOSA, N-MeFOSAA, NEtFOSAA, 4_2 FTS, 6_2 FTS, 8_2 FTS, ADONA, 9Cl-PF3ONS, 11Cl-PF3OUdS, GenX, 13C-PFBA, 13C5-PFPeA, 13C5-PFHxA, 13C4-PFHpA, 13C8-PFOA, 13C9-PFNA, 13C6-PFDA, 13C7PFUnDA, 13C-PFDoDA, 13C-PFDoDA, 13C2-PFTreDA, 13C2PFHxDA, 13C3-PFBS, 13C3-PFHxS, 13C8-PFOS, D5-NEtFOSAA, D3-N-MeFOSAA, 13C-FOUEA, 13C4-8:2 diPAP, 13C2-4:2 FTS, 13C2-6:2 FTS, 13C2-8:2 FTS, 13C-FHEA, 13CFOEA, 13C-FDEA, 13C3-GenX 11Cl-PF3OUdS, 9Cl-PF3ONS, ADONA, M2 4-2 FTS, M2 6-2 FTS, M2 8-2 FTS, M2PFDoA, M2PFOA, M3HFPO-DA, M3PFBS, M4PFBA, M4PFHpA, M5PFHxA, PFUnA, M8PFOA, M8PFOS, M9PFNA, M5PFPeA, m6PFDA, M4PFBA, PFBA, PFBS, PFDA, PFDoA, PFDS, PFEESA, PFHpA, PFHpS, 4-2 FTS, 6-2 FTS, 8-2 FTS, HFPO-DA-CO2, NDFHA, NDFHA-CO2, PFHxA, PFHxS, PFMBA, PFMPA, PFNA, PFOA, PFOS, PFPeA, PFPeS, PFUnA PFHxA, PFHpA, PFOA, PFDA, PFuDA, PFDoA, PFTrDA, PFTeDA, PFBS, PFHxS, PFOS, n-EtFOSAA, n-MeFOSAA FTA 6:2, FTA 8:2, FTA 10:2, N-MeFOSA, N-EtFOSA, NMeFOSE, N-EtFOSE PFBA, C4-PFBA, PFMPA, PFPeA, C6-PFPeA, PFBS, C3-PFBS, PFMBA, PFEESA, NFDHA, C6PFHxA, 4:2FTS, C2 4:2 FTS, PFHxA, C5-PFHxA, PFPeS, C3-PFHxS, HFPO-DA, C3-HFPO-DA, PFHpA, C4-PFHpA, PFHxS, ADONA, 6:2FTS, C2-6:2FTS, PFOA, C8-PFOA, PFHpS, PFNA, C9-PFNA, PFOS, C8-PFOS, 9ClPF3ONS, 8:2FTS, C2-8:2FTS, PFDA, C6-PFDA, PFUnA, C7PFUnA, 11Cl-PF3OUdS, PFDoA, C2-PFDoA na CAS (if available in source) na na na 29420-49-3, 3871-99-6, 1763-23-1, 757124-72-4, 27619-97-2, 39108-34-4, 706-91-4, 375-92-8, 68259-12-1, 2806-15-7, 375-22-4, 2706-90-3, 3024-4, 375-85-9, 335-67-, 375-95-1, 335-76-2, 2058-94-8, 307-55-1, 72629-94-8, 376-06-7, 2991-50-6, 2355-31-9, 754-91-6 na na na na 375-22-4, 2706-90-3, 307-24-4, 375-85-9, 33567-1, 375-95-1, 335-76-2, 2058-94-8, 307-55-1, 72629-9-8, 376-06-7, 67905-19-5, 16517-11-6, 29420-49-3, 2706-91-4, 3871-99-6, 375-92-8, 1763-23-1, N/A, 335-77-3, 2991-50-6, 2355-31-9, 70887-88-6, 70887-84-2, 678-41-1, 757124-72-4, 29420-49-3, 39108-34-4, 67584-42-3, 53826-123, 27854-31-5, 53826-13-4, 812-70-4, 95844544-8, 73606-19-6, 73606-19-6, 13252-13-6, 863090-89-5, 151772-58-6, 113507-82-7 375-22-4, 2706-90-3, 307-24-4, 375-85-9, 33567-1, 375-95-1, 335-76-2, 2058-94-8, 307-55-1, 72629-9-8, 376-06-7, 67905-19-5, 16517-11-6, 29420-49-3, 2706-91-4, 3871-99-6, 375-92-8, 1763-23-1, N/A, 335-77-3, 2991-50-6, 2355-31-9, 70887-88-6, 70887-84-2, 678-41-1, 757124-72-4, 29420-49-3, 39108-34-4, 67584-42-3, 53826-123, 27854-31-5, 53826-13-4, 812-70-4, 95844544-8, 73606-19-6, 73606-19-6, 13252-13-6, 863090-89-5, 151772-58-6, 113507-82-7 na na na na na na Sampling na sample amount used na na na Surface water, municipal wastewater, industrial wastewater, and groundwater samples 1000 mL reagent water, surface water, ground water, and waste water 5 mL A 10 g soil sample was in 250 mL polypropylene or polyethylene bottles 10 g na na serum na na na surface water, ground water, influent waste water, effluent waste water 250 mL surface water, ground water, influent waste water, effluent waste water 5 mL na water na na 250 mL na 1 g of cut textiles was weighed into a 20 mL glass vial and 10 mL of tetrahydrofuran (THF) was added na water 250 mL na na Pre- treatment Similar to previous EPA methods, water samples are concentrated using solid-phase extraction (SPE) cartridges, but the choice of cartridge is flexible and the sample volume can vary from 100-250 mL Methods follow those outlined in the EPA Method 533 document na Sample preparation was performed according to ISO 9562 na Sample clean-up used a styrene-divinylbenzene (SDVB) polymer SPE cartridge (500 mg, 6 mL), on a vacuumcontrolled manifold na : PFAS were extracted from 50 L serum samples by using a protein precipitation procedure Sample preparation and data processing were carried out according to EPA Method 537 prepared as mix in methanol ASTM 7979-17 spiked with 160 ng/L isotopically labeled IS na The samples were then extracted using SPE following the protocol described in the respective EPA methods Sample preservation and preparation were performed according to the guidelines in EPA Method 537.1 na na na Extraction na na na na na na na ISO 25101 Oasis WAX 6 cc, 150mg SPE na Oasis WAX na The water samples were extracted using the following procedure with Phenomenex Strata-XL solid phase extraction cartridges (6 mL, 500 mg): 1. Condition SPE tubes with 15 mL of water followed by 18 mL of methanol 2. Add sample to tubes at a flow rate of approximately 10-15 mL per minute. 3. Rinse tubes with 7.5 mL of water and repeat 4. Dry tubes under vacuum for 5 minutes 5. Rinse sample bottle with 4 mL of methanol and transfer methanol to SPE tube while collecting eluent and repeat 6. Evaporate sample to dryness under nitrogen at 40-60C 7. Reconstitute sample in 1 mL of 96% methanol 4% water containing 1 ng/L of internal standards 8. Transfer a 0.25 mL aliquot to a polypropylene vial and archive the remaining volume na na na Clean up na na na na na na na na na na na na na na na Measurement The SCIEX ExionLCTM system was used and chromatographic separation was achieved using gradient conditions with a Phenomenex Gemini C18 column (50 x 2 mm, 3 m particle size). A delay column was used to separate the instrument PFAS contamination from the analyte peak. The mobile phases were water (A, modified with 20 mM ammonium acetate) and methanol (B) with a flow rate of 0.6 mL/min. The column oven was 40oC and the injection volume was 2 L : Analysis was performed on the SCIEX 5500+ System with the Turbo VTM Ion Source using an electrospray ionization (ESI) probe in negative ion mode Agilent 1260 series Infinity Agilent 6470 Triple Quadrupole MS/MS with Agilent Jet Stream ESI source negative mode Analytical column Agilent ZORBAX Eclipse Plus C18, 3.0 50 mm; 1.8 m (p/n 959757-302) Delay column Agilent Eclipse Plus C18, 4.6 50 mm, 3.5 m (p/n 959943-902) Column temperature 50 C Injection volume 5 uL Mobile phase A) 5 mM Ammonium acetate in water (LC grade) B) 5 mM Ammonium acetate in 95 % MeOH (LC grade) Gradient flow rate 0.4 mL/min Gradient Time (min) %B 0.0 10 0.5 10 2.0 30 14.0 95 14.5 100 Stop time 16.5 minutes Post time 6 minutes Thermo ScientificTM DionexTM ICS-2100 Integrated Reagent-FreeTM Ion Chromatography (RFICTM) system Mitsubishi Chemical Analytech Automatic Combustion Unit Model AQF-2100H system Thermo ScientificTM DionexTM IonPacTM AS20 column, 2 250 mm Thermo ScientificTM DionexTM IonPacTM AG20 guard column, 2 50 mm KOH gradient Inject (0 min) 2 mM (0-0.1 min) 2-3 mM (0.1-5 min) 3-12 mM (5-21 min) 12 mM (21-24 min) 12-35 mM (24-25 min) 35 mM (25-28 min) 35-100 mM (28-28.2 min) 100 mM (28.2-32.2 min) 2 mM (32.2-32.4 min) 0,25 mL/min 250 l inj, temp: 30 C (column temperature) 35 C (detector cell temperature) Dionex AERS 500 suppressor (2 mm), timed constant current mode: 8 mA (0-28 min) 22 mA (28-33.2 min) 62 mA (33.2-37.4 min) 8 mA (37.4-44 min) the LC-MS/MS system comprised a Thermo ScientificTM VanquishTM Flex Binary UHPLC system fitted with a Thermo ScientificTM PFC-free kit (P/N 80100-62142) and interfaced with a Thermo ScientificTM TSQ AltisTM triple quadrupole mass spectrometer equipped with a HESI ionization probe. An isolator column was also installed after the LC pump and prior to the injection valve to offset background contaminants from the LC pump, Analytical column: Thermo ScientificTM AccucoreTM RP-MS, 2.6 m, 2.1 100 mm (P/N 17626-102130) Isolator column: Thermo ScientificTM HypersilTM BDS C18, 5 m, 2.1 50 mm (P/N 28105-052130) Column temp.: 45 C Flow rate: 0.5 mL/min Solvent A: Water containing 2 mM ammonium acetate, 2% methanol, and 0.1% acetic acid Solvent B: Methanol containing 2 mM ammonium acetate, 2% water, and 0.1% acetic acid Injection volume: 25 L Gradient: Time (min) % Solvent B 0 0 1 30 6 45 13 80 14 95 17 95 18 0 21 0 A Thermo ScientificTM VanquishTM LC, with all TeflonTM lines replaced by PEEK tubing, coupled to a Thermo ScientificTM TSQ QuantisTM triple quadrupole mass spectrometer, was used for sample analysis. Solvent B 10 mM ammonium acetate in 19% v/v acetonitrile/81% methanol Solvent A 10 mM ammonium acetate in 19% v/v acetonitrile in water Column temperature 25 C Gradient Solvent ramps from 40% Solvent B to 90% Solvent B over 15 min LC flow rate 0.300 mL/min Impurity Delay method. [HPLC conditions] (NexeraTM Series) Column : Shim-pack VeloxTM SP-C18 (150 mm L 2.1 mm I.D., 2.7 m, PN: 227-32003-04 Delay column : Shim-packTM XR-ODS (75 mm 2.0 mm I.D., 3 m, PN: 228-41623-91) Mobile phases : A) 20 mmol/L Ammonium Acetate in H2O B) Methanol Gradient program : B 60% (0.00 min) - B85% (25.00 - 30.00 min) - 60% (30.01 - 34.00 min) Flow rate : 0.25 mL/min Column temp. : 40 Injection volume : 50 L [MS conditions] LCMSTM-8060) Ionization : ESI (Negative mode) [HPLC conditions] (Nexera Series) Column : Shim-pack ODS (50 mm x 2.0 mm I.D., 1.6 m, P/N: 228-59922-91) Delay column : Shim-pack XR-ODS (30 mm x 3.0 mm I.D., 2.2 m, P/N: 228-41606-91) Mobile phases : A) 5mM Ammonium Acetate / 0.05% Acetic Acid in H2O B) Methanol Gradient program : B 50%(0.00 min) - B100%(4.60-5.50 min) Flow rate : 0.4 mL/min Column temp. : 40 Injection volume : 40 L [MS conditions] (LCMS-8050) Ionization : ESI (Negative mode) UHPLC separation was performed on a Phenomenex Gemini C18 column (50 x 2 mm, 3 m, 00B4439-B0) at 25C on a SCIEX ExionLCTM AC System. A Phenomenex Luna C18(2) column (30 x 2 mm, 5 m, 00A-4252Y0) was installed between the pump mixing chamber and the analytical column used for separation. The LC flow rate was 0.6 mL/min and the total run time was 6.5 min. The injection volume was 10 L : Data were collected using a SCIEX QTRAP 6500+ System with a IonDriveTMTurbo V Ion Source, operated with electrospray ionization (ESI) in negative mode. The microflow analysis was performed using an M5 MicroLC System at a flowrate of 10 L/min. A Gemini C18 3 m, 100 x 0.3 mm column (Phenomenex) was used. This column uses the identical stationary phase, but smaller internal diameter as the high flow method.5 Mobile phases A and B were Milli-Q water with 10 mM ammonium acetate and J.T.Baker Ultra LC-MS grade methanol with 10 mM ammonium acetate, respectively Time (Min) % Mobile Phase A % Mobile Phase B 0 98 2 1.2 45 55 7 1 99 8.5 0 100 8.6 98 2 The sample was injected into the SCIEX Triple Quad 6500+ System equipped with a OptiFlow Turbo V Ion Source that was designed specifically for lower flow rates. Waters Xevo TQ-S micro with PFC Analysis Kit. ESI- Acquity UPLC-IClass PLUS. Acquity UPLC BEH C18 2,1 x 100 mm, 1,7m. T: 35 C, sample T: 10 C, injection vol: 10 l, Mobile phase A: 95:5 Water: Methanol + 2 mM ammonium acetate; Mobile phase B: Methanol + 2mM ammonium acetate Gradient: 0 min: 0,3 ml/min 100% A, 1 min: 0,3 ml/min 800% A, 6 min: 0,3 ml/min 55% A, 13 min: 0,3 ml/min 20% A, 14 min: 0,4 ml/min 5% A, 17 min: 0,4 ml/min 5% A, 18 min: 0,3 ml/ min 100% A, 22 min: 0,3 ml/min 100% A Waters Xevo TQ-S micro with PFC Analysis Kit. ESI- Acquity UPLC-IClass PLUS. Acquity UPLC CSH Phenyl Hexyl 2,1 x 100 mm, 1,7m. T: 35 C, sample T: 10 C, injection vol: 30 l, Mobile phase A: 95:5 Water: Methanol + 2 mM ammonium acetate; Mobile phase B: Methanol + 2mM ammonium acetate Gradient: 0 min: 0,3 ml/min 100% A, 1 min: 0,3 ml/min 800% A, 6 min: 0,3 ml/min 55% A, 13 min: 0,3 ml/min 20% A, 14 min: 0,4 ml/min 5% A, 17 min: 0,4 ml/min 5% A, 18 min: 0,3 ml/min 100% A, 22 min: 0,3 ml/min 100% A Waters Xevo TQ-S micro with PFC Analysis Kit. ESI- Acquity UPLC-IClass PLUS. Acquity UPLC HSS T3 2,1 x 100 mm, 1,8m. T: 35 C, sample T: 4 C, injection vol: 5 l, Mobile phase A: 95:5 Water: Methanol + 2 mM ammonium acetate; Mobile phase B: Methanol + 2mM ammonium acetate Gradient: 0 min: 0,3 ml/min 100% A, 1 min: 0,3 ml/min 800% A, 6 min: 0,3 ml/min 55% A, 13 min: 0,3 ml/min 20% A, 14 min: 0,4 ml/min 5% A, 17 min: 0,4 ml/min 5% A, 18 min: 0,3 ml/ min 100% A, 22 min: 0,3 ml/min 100% A Agilent 1290 Infinity II, Agilent Ultivo triple quadrupole LC/MS Agilent Poroshell 120 EC-C18, 2.1 50 mm, 4 m (p/n 699770-902T) gilent Poroshell 120 EC-C18, 2.1 50 mm, 1.9 m (p/n 699675-902 55C A: 0,1% Acetic acid in H2O, B: Methanol injection 4 ul, flow rate 0,7 mL/min A: 20mM Ammonium acetate in H2O, B: Methanol, injection 7ul, flow 0,7 mL/min : An Agilent 1200 binary pump was modified by replacing all clear fluoroethylene polymer (FEP) tubing with 1/8 in or 1/16 inch PEEK tubing. A delay column (Phenomenex Luna C18(2), 5m, 30x2mm) was inserted between the gradient mixing chamber and the autosampler valve to retain contaminants from the eluents or pumps for an extra 1-2 min compared with target analytes eluting from the analytical column. An Agilent 1200 autosampler injected 10 ul of each sample onto the analytical column (Phenomenex Gemini C18, 3m, 50x2mm), which was heated to 40C. Gradient separation was performed at a flow rate of 0.6 mL/min Mobile phase A - 20 mM ammonium acetate Mobile phase B - methanol 0 min: 95%A; 0,1 min, 45% A; 4,5 min: 1% A; 8 min: 1% A; 8,5 min: 95% A : Samples were ionized using negative mode electrospray For the PCI-SIM method, a single quadrupole GC/MS, GCMS-QPTM 2020 NX was used. A triple quadrupole GC-MS/MS system, GCMS-TQTM8050 NX, was used for the EI-MRM method. The same GC conditions were applied to both methods GC-MS : GCMS-QP2020 NX and GCMS-TQ8050 NX Auto-Injector : AOCTM-20i + 20s Column : SH-RtxTM-200 (length 30 m, 0.32 mm I.D., _x001E_lm thickness 0.5 m) [GC] Injection Temp. : 250 C Column Oven Temp. : 80 C => (30 C /min) => 260 C (1 min) Injection Mode : Splitless Carrier Gas : He Carrier Gas Control : 48.7 cm/sec (Constant Velocity) High Pressure Injection : 150 kPa (1 min) Injection Volume : 2 L [MS] Ion Source Temp. : 200 C Interface Temp. : 250 C EI-MRM Ionization Mode : EI Acquisition Mode : MRM Event Time : 0.3 sec PCI-SIM Ionization Mode : PCI Acquisition Mode : SIM Reagent Gas : Methane (200 kPa) Event Time : 0.1 sec Thermo ScientificTM DionexTM AutoTraceTM 280 PFAS, Thermo ScientificTM VanquishTM Flex UHPLC system, Thermo ScientificTM TSQ FortisTM triple quadrupole mass spectrometer Thermo ScientificTM VanquishTM system fitted with Thermo ScientificTM PFC-free kit Thermo ScientificTM AcclaimTM 120 C18 column, 2.1 150 mm, 2.2 m Thermo ScientificTM HypersilTM BDS C18 column, 2.1 50 mm, 5 m Column temperature 45 C Injection volume 5 uL Mobile phase A) 20 mM ammonium acetate B) Methanol t:0 min, %B 5 flow 0,4 mL/min; t:0,5 min, %B 5 flow 0,4 mL/min; t:3 min, %B 40 flow 0,4 mL/min; t:14 min, %B 85 flow 0,4 mL/min; t:17 min, %B 85 flow 0,4 mL/min; t:18 min, %B 5 flow 0,4 mL/min t:21 min, %B 5 flow 0,4 mL/min Sensors are used for detection of PFAS: nanoparticle based sensor, electrochemical sensor, fluorescence detector and smartphone based sensor analytical methods for detecton of PFAS: TOP assay, total fluorine content - CIC (EOF and AOF), LC-MS and GC-MS Quantification method na Working range (ng/mL) As na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na na Matrices reported levels (ng/mL) na na na na Surface water between 4.5 and 10.2 g/L, Groundwater samples n 2 and 7 g/L Municipal sewage treatment plants 2 and 8.5 g/L Industrial wastewater values above 74 g/L, with a highest value of na more than 500 g/L na na na na na na na na The concentrations of PFBS ranged from 0.5 to 44.8 ppt in the samples before extraction. PFOS was the second most detected compound, present in 8 of 20 samples, with concentrations ranging from 1.9 ppt to above the na ULOQ surface water, ground water, influent waste water, effluent waste water 0,1-50 (PFPeA) ng/L surface water, ground water, influent waste water, effluent waste water 10-8000 ng/L human serum Total: 8,86-19 ng/L na na na na Textile The detected and quantitated concentrations of N-MeFOSE was 1.74 ng/g and that of N-EtFOSE was 2.91 ng/g FTA 8:2 and FTA 10:2 were quantitated to be 89.8 ng/g and 41.0 ng/g, respectively na na na na info - validation of the method Limitations Calibration curve linearity was excellent with r2 values greater than 0.999 for most PFAS compounds over the 0.5-100 ng/mL standard range s the accuracy was very good, generally 100% +/- 5% (Figure 6). Precision was also very good, the CV% was ~5% for the 0.5 ng/mL standard and ~2% for the 25 ng/m na e linearity, accuracy 76 % to 120 %, precision 4-15%, and instrument detection limits 0.02 ng/L na e linearity of the calibration function within the range of 2 to 500 g/L Recovery ranged from 16% to 121% The wastewater matrix showed recoveries from 85% to 102% na Excellent linearity and quantitative accuracy were achieved over the range of 5 to 200 ng/L All compounds analyzed in this method were within the range of 70% to 130% na Recovery: 71-110 % na e calibration curves for both PFOA and PFOS indicate good linearity with R2 > 0.999 The accuracy of the calibration curve was 91.4 to 101.5%, which is a good result. Figure 3 shows each chromatogram of the 1 ng/L standard sample for PFOA and PFOS, respectively. The repeatability (n = 3) of the standard sample at this concentration was 5.8% for PFOA and 4.9% for PFOS, indicating good reproducibility. na Method demonstrated excellent reproducibility and linearity for PFAS concentrations ranging from 0.5 to 100 ng/mL, with R2 values greater than 0.99, while maintaining accuracy and precision across the calibration range inter-day peak area variations of 5% or less na Using the outlined method, PFBS and PFHxA met all asymmetry requirements with values ranging from 1.0 to 1.2 (Table 3) at all the quality control concentration levels. Additionally, the ion ratios for both PFBS and PFHxA were within 20% and the calculated concentration was within 5% of the expected value The mean ISTD area was calculated and all collected data points fell within 20%, suggesting no major suppression was occurring. The surrogate concentrations were also plotted over the 3 day run and found to be within the acceptable 30% outlined in EPA Method 537 na Linearity, Recovery: 75-130%, Repeatability RSD: <15%, Robustness RSD: <10% na Linearity, Recovery: 70-130%, Repeatability RSD: <10%, na Linearity, residuals <15%, accuracy <20% na 4. Recoveries were well within the 70 to 130% range required by the EPA methods. The RSDs were <20% na 1. Linearity (r2>0.99) (as shown in Figure 2) 2. Accuracy (+/- 30% for each calibrator) 3. Precision (RSD <20% of 4 replicates of a fortified blank) 4. Asymmetry factor (>0.8 and <1.5 for the first 2 peaks in the chromatogram as shown in Figure 3) 5. Surrogate recovery +/- 30% of expected response 6. Laboratory reagent blanks (LFBs) and field reagent blanks (FRBs) quantitated at <1/3 of the MRL. na The four identification points were: (1) 0.10 min deviation of absolute retention time (2) 1 quantitative or target MRM transition (3) 2 product ions (i.e. at least 1 qualitative or reference MRM transition) (4) The maximum tolerances for relative intensity% of reference MRM Linear IS calibration curves with average R2 0.998 were obtained. Repeatability of the peak area ratios were evaluated at the lowest, mid and highest calibration levels from six replicates (Table 5). The %RSD at the lowest calibration levels of all targets ranged from 3.54 to 17.2%. the QC samples were quantitated to be in the range of approx. 30% of the spiked concentrations na within 70-130% of their true value, calculated RSDs were all less than 20% na na na LoD (ng/mL) subgroup Measurement - generic name 2 ng/L na LC-MS/MS 0,02 ng/L na LC-MS/MS 1.3 g/L na LC-MS/MS 1 ng/L na LC-MS/MS 0,01 ng/g na LC-MS/MS 1 ng/L na LC-MS/MS 0,1 ng/mL na LC-MS/MS The lower limit of quantification (LLOQ) varied between 1 and 5 parts per trillion (ppt) in vial, equating to 0.04 and 0.2 ppt in the sample before extraction na LC-MS/MS LOD: 2 (PFOA) - 2000 (PFOcDA), most 10 ng/L in vial and 0,01 - 8, most 0,04 ng/L in sample na LC-MS/MS LOD: 0,82 (ADONA) - 7948 (FDEA) ng/L na LC-MS/MS 0,05 - 20 ng/mL na LC-MS/MS 0,13-0,92 ng/L na LC-MS/MS 0,2 ng/L na LC-MS/MS 0.5 - 4 ng/mL na GC-MS 2 to 10 ng/L na LC-MS/MS nanoparticle based sensors (2.5 ng/L LOD) electrochemical sensor (30 g/L LOD) fluorescence detector (124 g/L PFOA LOD) na sensor, TOPassay, CIC, LC-MS/MS, GC-MS